Acetyl chloride → HCID 46938718、化合物

HRID 1866554ノート

反応式

HRID 1866554 の反応式
[C:1](Cl)(=O)C.ClCC([NH:9][C:10]([CH3:23])([CH3:22])[CH2:11][C:12]1[CH:13]=[C:14]([CH2:18][C:19]([OH:21])=[O:20])[CH:15]=[CH:16][CH:17]=1)=O>CO>[CH3:1][O:21][C:19](=[O:20])[CH2:18][C:14]1[CH:15]=[CH:16][CH:17]=[C:12]([CH2:11][C:10]([NH2:9])([CH3:23])[CH3:22])[CH:13]=1

参加物

4

反応物 2

HCID 6367Acetyl chlorideHCID 46938812{3-[2-(2-Chloroacetamido)-2-methylpropyl]phenyl}acetic acid

生成物 1

HCID 46938718HCID 46938718、化合物収率 87%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Acetyl chloride (154.5 g, 1.97 mol) was added to a solution of {3-[2-(2-chloro-acetylamino)-2-methyl-propyl]-phenyl}-acetic acid (preparation 48), (20 g, 0.66 mol) in methanol (350 mL) and the mixture was heated under reflux for 18 hours. The reaction mixture was then concentrated in vacuo to afford the title compound as a brown oil in 87% yield, 154.5 g. 1H NMR (300 MHz, CDCl3) δ: 7.22 (1H, m), 7.18-7.05 (3H, m), 3.71 (3H, s), 3.58 (2H, s), 2.62 (2H, s), 1.12 (6H, s) ppm; GCMS m/z 206 [M−H]−.

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 18 hours
  3. concentrationThe reaction mixture was then concentrated in vacuo

出典と根拠

ORDレコード
ord-702ef986f5884c35bdea60c00ed69659
出典データセット
uspto-grants-2009_12
特許番号
US07629358B2

反応ノート

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