Acetic Anhydride → HCID 44185486, 화합물

HRID 241426노트

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HRID 241426 반응식
[C:1]([O:4][C:5](=O)C)(=O)[CH3:2].[F:8][CH:9]([F:18])[C:10](=[O:17])[CH2:11][C:12]([O:14][CH2:15][CH3:16])=[O:13].C(OCC)(OCC)OCC>>[CH2:1]([O:4]/[CH:5]=[C:11](/[C:10](=[O:17])[CH:9]([F:18])[F:8])\[C:12]([O:14][CH2:15][CH3:16])=[O:13])[CH3:2]

참가 물질

4

반응물 3

HCID 7918Acetic AnhydrideHCID 31214Ethyl orthoformateHCID 67697Butanoic acid, 4,4-difluoro-3-oxo-, ethyl ester

생성물 1

HCID 44185486HCID 44185486, 화합물수율 86%

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온도
95 °C

실험 절차

Add acetic anhydride (166 kg, 1625 mol) to a mixture of ethyl 4,4-difluoroacetoacetate (33 kg, 199 mol) and triethyl orthoformate (60 kg, 407 mol) maintained at 90-100° C. Stir the mixture at 90-100° C. for 8.5 hours and remove ethyl acetate using a Dean-Stark apparatus. Concentrate the reaction mixture to give the title compound (37.8 kg, 86% yield, 97% GC purity). 1H NMR (500 MHz, CDCl3,) δ 7.88 (d, J=6 Hz, 1H), 6.3 (m, 1H), 4.3 (m, 4H), 1.4 (m, 3H), 1.32 (m, 3H).

후처리

  1. customremove ethyl acetate using a Dean-Stark apparatus
  2. concentrationConcentrate the reaction mixture

출처 및 근거

ORD 기록
ord-2f31eeba3ae24037aa384e57ebfa7c2f
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08648200B2

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