Acetic Anhydride → 2-thiocyanatoethyl acetate
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[S-:1][C:2]#[N:3].[C:4]([O:7][C:8](=O)[CH3:9])(=[O:6])[CH3:5]>N1C=CC=CC=1.ClCCl>[C:4]([O:7][CH2:8][CH2:9][S:1][C:2]#[N:3])(=[O:6])[CH3:5]참가 물질
실험 절차
A mixture of 2-bromoethanol (7.0 g) and potassium thiocyanate (5.4 g) in methanol (40 ml) was refluxed for 7 hours. After precipitate was filtered off, the filtrate was evaporated under reduced pressure. The residue was suspended in chloroform/methanol (5/1). The precipitate was filtered off. The filtrate was evaporated under reduced pressure to give the thiocyanate (4.4 g). To a mixture of the thiocyanate in pyridine (4.8 ml)/dichloromethane (20 ml) was added acetic anhydride (5.3 ml) in dichloromethane (5 ml) at 5° C. The mixture was stirred at room temperature for 6 hours. The precipitate was filtered off. The filtrate was washed with water, dried over sodium sulfate and evaporated under reduced pressure to give 2-thiocyanatoethyl acetate (5.6 g).
후처리
- filtrationThe precipitate was filtered off
- washThe filtrate was washed with water
- dry with materialdried over sodium sulfate
- customevaporated under reduced pressure
출처 및 근거
- ORD 기록
- ord-f271f7cbb72c49e5987e2aedb10e3a54
- 출처 데이터셋
- uspto-grants-2011_04
- 특허 번호
- US07928264B2
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