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Acetic Anhydride → HCID 53655523, 화합물

HRID 1788976
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HRID 1788976 반응식
[F:1][C:2]1[C:12]([F:13])=[C:11]([F:14])[C:10]([F:15])=[CH:9][C:3]=1[C:4]([CH2:6][C:7]#[N:8])=[O:5].[CH:16]([O-])([O-])[O:17][CH2:18][CH3:19].C(OC(=O)C)(=O)C>>[CH2:18]([O:17][CH:16]=[C:6]([C:4](=[O:5])[C:3]1[CH:9]=[C:10]([F:15])[C:11]([F:14])=[C:12]([F:13])[C:2]=1[F:1])[C:7]#[N:8])[CH3:19]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 7918Acetic AnhydrideHCID 139117863-Oxo-3-(2,3,4,5-tetrafluorophenyl)propanenitrileHCID 53630039Ethylorthoformate

생성물 1

HCID 53655523HCID 53655523, 화합물수율 88%

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온도
100 °C

실험 절차

A mixture of 2-(2,3,4,5-tetrafluorobenzoyl)acetonitrile (13.1 g), ethyl orthoformate (13.4 g) and acetic anhydride (15.4 g) is heated at 100° C. with stirring for 3 hours. The reaction mixture is concentrated under vacuum to yield an orange brownish oily residue. When the oily residue is allowed to stand at room temperature, it crystallizes slowly. The resulting crystals are collected and washed successively with a 2:1 mixture of hexane and ethyl acetate, and a 5:1 mixture of hexane and ethyl acetate to give 3-ethoxy-2-(2,3,4,5-tetrafluorobenzoyl)acrylonitrile (14.5 g) as light orange crystals, m.p. 99°-101° C.

후처리

  1. concentrationThe reaction mixture is concentrated under vacuum
  2. customto yield an orange brownish oily residue
  3. customto stand at room temperature
  4. customit crystallizes slowly
  5. customThe resulting crystals are collected
  6. washwashed successively with a 2:1 mixture of hexane and ethyl acetate
  7. additiona 5:1 mixture of hexane and ethyl acetate

출처 및 근거

ORD 기록
ord-f4e9bacf1cdc4752baaef28e79f8c8f7
출처 데이터셋
uspto-grants-1987_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04686221

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