Methyl acetoacetate → ST50708819

HRID 2254130노트

반응식

HRID 2254130 반응식
[F:1][C:2]([F:12])([F:11])[C:3]1[CH:10]=[CH:9][C:6]([CH:7]=O)=[CH:5][CH:4]=1.[C:13]([O:19][CH3:20])(=[O:18])[CH2:14][C:15]([CH3:17])=O.Cl.[CH3:22][NH2:23]>N1C=CC=CC=1>[CH3:22][N:23]1[C:15]([CH3:17])=[C:14]([C:13]([O:19][CH3:20])=[O:18])[CH:7]([C:6]2[CH:9]=[CH:10][C:3]([C:2]([F:12])([F:11])[F:1])=[CH:4][CH:5]=2)[C:14]([C:13]([O:19][CH3:20])=[O:18])=[C:15]1[CH3:17]

참가 물질

5

반응물 3

HCID 7757Methyl acetoacetateHCID 679964-(Trifluoromethyl)benzaldehydeHCID 6364545Methylamine hydrochloride

생성물 1

HCID 2167221ST50708819

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

A mixture of 5.22 g (0.03 mol) of 4-trifluoromethylbenzaldehyde, 7.04 g (0.06 mol) of methyl acetoacetate and 2.07 g (0.03 mol) of methylamine hydrochloride in 20 ml of pyridine is stirred under reflux for 5 hours. After removing the pyridine by distillation, the mixture is partitioned between water and methylene chloride, and the organic phase is washed with water, dried over sodium sulphate and evaporated. The residue is recrystallized from methanol.

후처리

  1. temperatureunder reflux for 5 hours
  2. customAfter removing the pyridine
  3. distillationby distillation
  4. customthe mixture is partitioned between water and methylene chloride
  5. washthe organic phase is washed with water
  6. dry with materialdried over sodium sulphate
  7. customevaporated
  8. customThe residue is recrystallized from methanol

출처 및 근거

ORD 기록
ord-ded9fdedfd2c4523ba39bc8f6b90dfed
출처 데이터셋
uspto-grants-1993_08
특허 번호
US05234935

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