Methyl acetoacetate → ST50708819

HRID 2254130ノート

反応式

HRID 2254130 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 2167221ST50708819

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ded9fdedfd2c4523ba39bc8f6b90dfed
出典データセット
uspto-grants-1993_08
特許番号
US05234935

反応ノート

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