Triethylamine → 2-Bromo-4,4,4-trifluorocrotononitrile

HRID 974405노트

반응식

HRID 974405 반응식
C(N(CC)CC)C.[Br:8][CH:9]([CH:12](Br)[C:13]([F:16])([F:15])[F:14])[C:10]#[N:11]>O1CCCC1>[Br:8]/[C:9](=[CH:12]\[C:13]([F:16])([F:15])[F:14])/[C:10]#[N:11]

참가 물질

4

반응물 2

HCID 8471TriethylamineHCID 109020202,3-Dibromo-4,4,4-trifluorobutyronitrile

생성물 1

HCID 218608782-Bromo-4,4,4-trifluorocrotononitrile수율 82%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Triethylamine (3.7 g, 0.037 mol) is added dropwise to a solution of 2,3-dibromo-4,4,4-trifluorobutyronitrile (5.32 g, 0.023 mol) and tetrahydrofuran (100 mL). A voluminous white precipitate forms during the addition. Stirring is continued for 1 hour, then the solid is filtered off and washed with tetrahydrofuran. The tetrahydrofuran is distilled off to give a dark brown oil. Bulb to bulb distillation (15 mm, 24° C.) of the oil yields the title product as a clear colorless liquid (3.1 g, 82%). NMR spectral analyses identifies a 6:1 mixture of E:Z.

후처리

  1. additionA voluminous white precipitate forms during the addition
  2. filtrationthe solid is filtered off
  3. washwashed with tetrahydrofuran
  4. distillationThe tetrahydrofuran is distilled off
  5. customto give a dark brown oil
  6. distillationBulb to bulb distillation (15 mm, 24° C.) of the oil

출처 및 근거

ORD 기록
ord-b9f0e5d14d7944e6977df5a35666a36d
출처 데이터셋
uspto-grants-1991_11
특허 번호
US05068390

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