Acetic Anhydride → HCID 70529331, 화합물

HRID 128169

반응식

HRID 128169 반응식
[F:1][C:2]1[CH:12]=[CH:11][C:5]([C:6]([CH2:8][C:9]#[N:10])=[O:7])=[CH:4][CH:3]=1.[C:13](OCC)(OCC)([O:15][CH2:16][CH3:17])[CH3:14].C(OC(=O)C)(=O)C>>[F:1][C:2]1[CH:3]=[CH:4][C:5]([C:6](/[C:8](=[C:13](/[O:15][CH2:16][CH3:17])\[CH3:14])/[C:9]#[N:10])=[O:7])=[CH:11][CH:12]=1

참가 물질

4

반응물 3

HCID 7918Acetic AnhydrideHCID 66221Triethyl orthoacetateHCID 2783172p-Fluorobenzoylacetonitrile

생성물 1

HCID 70529331HCID 70529331, 화합물

실험 절차

A solution of 16.3 g. of p-fluorobenzoylacetonitrile and 18.3 ml. of triethyl orthoacetate in 35 ml. of acetic anhydride is heated on a steam bath for 2.5 hours. The solvents are removed in vacuo and the residue is distilled at 165°-167° C./300μ. Upon cooling, this distillate solidifies and is recrystallized from methylene chloride/hexane to give the desired 2-(p-fluorobenzoyl)-3-ethoxycrotononitrile, m.p. 77°/89° C.

후처리

  1. customThe solvents are removed in vacuo
  2. distillationthe residue is distilled at 165°-167° C./300μ
  3. temperatureUpon cooling
  4. customthis distillate solidifies and is recrystallized from methylene chloride/hexane

출처 및 근거

ORD 기록
ord-ea48427f139844aca6b6b4feacd5221b
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04259256

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