Acetyl chloride → HCID 46938718, 화합물

HRID 1866554노트

반응식

HRID 1866554 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 46938718HCID 46938718, 화합물수율 87%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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]−.

후처리

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

출처 및 근거

ORD 기록
ord-702ef986f5884c35bdea60c00ed69659
출처 데이터셋
uspto-grants-2009_12
특허 번호
US07629358B2

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