Chlorosulfonyl isocyanate → HCID 14722020, 화합물
반응식
Cl[S:2]([N:5]=[C:6]=[O:7])(=[O:4])=[O:3].[CH3:8][O:9][C:10]1[CH:19]=[CH:18][CH:17]=[C:12]([C:13]([O:15][CH3:16])=[O:14])[C:11]=1[OH:20]>C1(C)C(C)=CC=CC=1>[CH3:16][O:15][C:13](=[O:14])[C:12]1[CH:17]=[CH:18][CH:19]=[C:10]([O:9][CH3:8])[C:11]=1[O:20][S:2]([N:5]=[C:6]=[O:7])(=[O:4])=[O:3]참가 물질
4
반응 조건
- 온도
- 140 °C
실험 절차
3.4 g (0.024 mol) of chlorosulfonyl isocyanate are added dropwise to a solution of 3.6 g (0.02 mol) of methyl 3-methoxy-salicylate in 20 ml of xylene at 25° C. When the dropwise addition has ended, the temperature is slowly increased to 140° C. and the mixture is heated under reflux for 2.5 hours. It is cooled and the solvent and excess chlorosulfonyl isocyanate are removed on a rotary evaporator. The yellow oil which remains (5.4 g=1004 of theory) is used without further purification.
후처리
- additionWhen the dropwise addition
- temperaturethe mixture is heated
- temperatureunder reflux for 2.5 hours
- temperatureIt is cooled
- customthe solvent and excess chlorosulfonyl isocyanate are removed on a rotary evaporator
- customis used without further purification
출처 및 근거
- ORD 기록
- ord-acdd9fd9f7d44198b26daaec0a1a2fd4
- 출처 데이터셋
- uspto-grants-1993_12
- 특허 번호
- US05272129
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