Methanol → 3-Methoxyisophthalaldehydic acid methyl ester

HRID 1111758노트

반응식

HRID 1111758 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 diisobutylaluminum hydride as a 1M 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-7e28c598cd014eee96c8a4e619016065
출처 데이터셋
uspto-grants-1978_10
특허 번호
US04118559

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