Triethylamine → HCID 23035382、化合物
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
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
- additionUpon completion of addition the reaction mixture
- washThe reaction mixture was then washed in succession with one 25 ml portion of water, two 25 ml portions of aqueous 5% sodium hydroxide
- dry with materialThe organic layer was dried with sodium sulfate
- filtrationfiltered
- 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
読み込み中…