Water → HCID 68587480、化合物

HRID 2070236ノート

反応式

HRID 2070236 の反応式
[C:1]([C:5]1[CH:6]=[C:7]([OH:11])[CH:8]=[CH:9][CH:10]=1)([CH3:4])([CH3:3])[CH3:2].Cl[C:13]1[C:18]([C:19]([F:22])([F:21])[F:20])=[CH:17][C:16]([N+:23]([O-:25])=[O:24])=[C:15]([CH3:26])[CH:14]=1.C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[C:1]([C:5]1[CH:6]=[C:7]([CH:8]=[CH:9][CH:10]=1)[O:11][C:13]1[C:18]([C:19]([F:20])([F:22])[F:21])=[CH:17][C:16]([N+:23]([O-:25])=[O:24])=[C:15]([CH3:26])[CH:14]=1)([CH3:4])([CH3:2])[CH3:3]

参加物

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 11450Phenol, 3-(1,1-dimethylethyl)-HCID 210179751-Chloro-5-methyl-4-nitro-2-(trifluoromethyl)benzene

生成物 1

HCID 68587480HCID 68587480、化合物収率 72%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

In 50 ml of N,N-dimethylformamide, 3.00 g (19.97 mmol) of 3-tertbutylphenol, 4.35 g (18.16 mmol) of 4-chloro-5-trifluoromethyl-2-methylnitrobenzene and 3.26 g (23.60 mmol) of potassium carbonate are heated at 50° C. for 15 min. The reaction solution is added to water and extracted repeatedly with dichloromethane, the extracts are dried over Na2SO4 and filtered and the solvent is removed under reduced pressure. The solid is washed with water and hexane and dried under reduced pressure. (6.6 g, purity 70.0%, yield 72.0%, log P (pH 2.3)=5.68).

後処理

  1. extractionextracted repeatedly with dichloromethane
  2. dry with materialthe extracts are dried over Na2SO4
  3. filtrationfiltered
  4. customthe solvent is removed under reduced pressure
  5. washThe solid is washed with water and hexane
  6. customdried under reduced pressure

出典と根拠

ORDレコード
ord-51a2b8c425b44971bcf466b0d7d814bf
出典データセット
uspto-grants-2012_10
特許番号
US08299301B2

反応ノート

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