Methanol → 3-Methoxyisophthalaldehydic acid methyl ester

HRID 225182노트

반응식

HRID 225182 반응식
C[C:2]1[C:3]([O:15][CH3:16])([C:12](O)=[O:13])[CH:4](C)[C:5](=[CH:9][CH:10]=1)[C:6]([OH:8])=[O:7].[H-].[CH2:18]([Al+]CC(C)C)C(C)C.CO>C1(C)C=CC=CC=1.CCCCCC>[CH3:18][O:8][C:6](=[O:7])[C:5]1[CH2:4][C:3]([O:15][CH3:16])([CH:2]=[CH:10][CH:9]=1)[CH:12]=[O:13]

참가 물질

6

반응물 3

HCID 887MethanolHCID 21225700DiisobutylaluminumhydrideHCID 86736056Dimethyl 3-methoxyisophthalic acid

생성물 1

HCID 867360553-Methoxyisophthalaldehydic acid methyl ester

시약·촉매·용매 2

HCID 1140Toluene용매HCID 8058Hexane용매

실험 절차

To a -78° C. to -100° C. solution of 1.0 mole of dimethyl 3-methoxyisophthalic acid in 5 liters of toluene is slowly added 1.0 mole of diisobutyl-aluminum hydride as a 1 M solution in n-hexane (reaction t≤-78° C.). The reaction mixture is stirred for 3 hours following the addition and is then quenched by the addition of 10 moles of anhydrous methanol. The reaction mixture is allowed to warm to room temperature and is stirred until a filterable precipitate forms. The reaction mixture is filtered and the filtrate evaporated. The residue is purified by vacuum distillation to yield 3-methoxyisophthalaldehydic acid methyl ester.

후처리

  1. customTo a -78° C. to -100° C.
  2. additionthe addition
  3. stirringis stirred until a filterable precipitate forms
  4. filtrationThe reaction mixture is filtered
  5. customthe filtrate evaporated
  6. distillationThe residue is purified by vacuum distillation

출처 및 근거

ORD 기록
ord-ea9c20a5e7244471a986200fba0fc9e7
출처 데이터셋
uspto-grants-1980_11
특허 번호
US04235913

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