2,22二羟甲基丁酸的制备工艺

2962002JOURNALOFBEIJINGUNIVERSITYOFCHEMICALTECHNOLOGYVol.29,No.620022,22(,100029):,,2,22,,2,22(IR)(NMR)():2,22;2,22;;:O62113+6:2002203220::,1974,,,2,22,,,2,22[1]2,22,[24],,,,1111,;3710%4010%,30%,,,,Nicolet210FTIR;ar400;1122,22[24],1mol212mol,40,,6h,2,221132,221mol2,22,2,223,70,112mol,8h,,,2,2222,22:CH3CH2CH2CHO+2HCHOAldolCH3CH2C(CH2OH)2CHO[O]CH3CH2C(CH2OH)2COOH21121111(1)1/2,22Table1Effectofmolarratioofformaldehydetobutyraldehydeonyieldof2,22dimethylolbutyraldehyden()/n()/%21011072162111107813212110851821311071142141106613,1,/210110212110,,/212110,,,21112(2)22,22Table2Effectofreactiontemperatureonyieldof2,22dimethylolbutyraldehydeT//%4078134588105079105570102,,,,45,,,,,45212212112,22(3)3/2,222,22Table3Effectofmolarratioofhydrogenperoxideto2,22dimethylolbutyraldehydeonyieldof2,22dimethylol2butyricacidn()/n(2,22)/%110110611711111067121121107712113110661711411054143,,,,22,,,,2,22,n()/n(2,22)112110,11211021212(4)2,22,,,,,,,42,22Table4Effectofvolumeratioofwaterto2,22dimethylolbu2tyraldehydeonyieldof2,22dimethylolbutyricacidV()/V(2,22)/%216614317612416819516810,2,22,,2,22,,,,,,,,,,21213(5)52,22Table5Effectofreactiontemperatureonyieldof2,22dimethylolbutyricacidT//%6065137075168075189064125,7080,,2,22,,,,,,,,,,,,21214(6)2,22,,;,2,22,2,22,48200262,22Table6Effectofreactiontimeonyieldof2,22dimethylolbu2tyricacidt/h2,22/%765138781997418106612,,,OO,,,2132,22IR(KBr,1),14571378cm-1,33301055cm-1,333016921246cm-112,22Fig.1IRspectrumof2,22dimethylolbutyricacid13C2NMR(DMSO,2),=81287,=221161,=39,=521766,=60147,=175195222,2213C2NMRFig.213C2NMRspectrumof2,22dimethylolbutyricacid32,22:212110,45;2,22:112110,2,223,7080,8h,2,227819%[1].2,22[J].,2000,8(18):30[2],.2,22[P].,112228478.1999208224[3],.2,22[P].,112228490.1999208224[4],.2,22[P].,112130719.1999205218Preparationof2,22dimethylolbutyricacidLIGai2yunSHIHong2yueZHANGJia2xinLIUYi2lingXUEChuan2xin(CollegeofScience,BeijingUniversityofChemicalTechnology,Beijing100029,China)Abstract:Usinginorganicbaseasacatalyst,2,22dimethylolbutyraldehydewaspreparedbythealdolcondensa2tionfromformaldehydeandbutyraldehyde.Then,takinghydrogenperoxideasanoxidant,2,22dimethylolbu2tyricacidwasobtained.Thereactionconditionsincludingmolarratio,reactiontime,solventandreactiontem2peraturewereinvestigated.ThestructureoftheproductwasconfirmedbyIRandNMR.Keywords:2,22dimethylolbutyraldehyde;2,22dimethylolbutyricacid;aldolcondensation;oxidation()586:2,22