Triethylamine → HCID 23035382、化合物

HRID 1710012ノート

反応式

HRID 1710012 の反応式
Cl.[NH2:2][CH2:3][CH2:4][C:5]([F:9])=[C:6]([F:8])[F:7].[C:10](Cl)(Cl)=[S:11].C(N(CC)CC)C>C(Cl)(Cl)Cl>[F:9][C:5](=[C:6]([F:8])[F:7])[CH2:4][CH2:3][N:2]=[C:10]=[S:11]

参加物

5

実験手順

To a stirred solution of 0.4 gram (0.0027 mole) of 4-amino-1,1,2-trifluoro-1-butene hydrochloride in 15 ml of chloroform was added 0.3 gram (0.003 mole) of thiophosgene, followed by 0.7 ml (0.009 mole) of triethylamine. Upon completion of addition the reaction mixture was stirred at ambient temperature for three hours. The reaction mixture was then washed in succession with one 25 ml portion of water, two 25 ml portions of aqueous 5% sodium hydroxide, and, finally, one 25 ml portion of water. The organic layer was dried with sodium sulfate and filtered. The filtrate was concentrated under reduced pressure to give 0.3 gram of (3,4,4-trifluoro-3-butenyl) isothiocyanate as an oil. The ir spectrum was consistent with the proposed structure.

後処理

  1. additionUpon completion of addition the reaction mixture
  2. washThe reaction mixture was then washed in succession with one 25 ml portion of water, two 25 ml portions of aqueous 5% sodium hydroxide
  3. dry with materialThe organic layer was dried with sodium sulfate
  4. filtrationfiltered
  5. concentrationThe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-a636f25a0fe04187a37199838424d985
出典データセット
uspto-grants-1990_08
特許番号
US04952580

反応ノート

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