1-Chloroethyl chloroformate → HCID 68578547、化合物
反応式
C([N:8]1[CH2:14][C:13]2[CH:15]=[CH:16][C:17]([F:22])=[C:18]([CH:19]3[CH2:21][CH2:20]3)[C:12]=2[O:11][CH2:10][CH2:9]1)C1C=CC=CC=1.[Cl:23]C(OC(Cl)C)=O>C1(C)C=CC=CC=1>[ClH:23].[CH:19]1([C:18]2[C:12]3[O:11][CH2:10][CH2:9][NH:8][CH2:14][C:13]=3[CH:15]=[CH:16][C:17]=2[F:22])[CH2:21][CH2:20]1参加物
4
反応条件
- 温度
- 80 °C
実験手順
A solution of 4-benzyl-9-cyclopropyl-8-fluoro-2,3,4,5-tetrahydro-1,4-benzoxazepine (408 mg, 1.37 mmol) and 1-chloroethyl chloroformate (0.178 ml, 1.65 mmol) in toluene (10 ml) was stirred at 90° C. for 2 hr, and the solvent was evaporated under reduced pressure. Methanol (10 ml) was added to the residue, the mixture was stirred at 80° C. for 1 hr, and diisopropyl ether (10 ml) was added. The precipitate was collected by filtration and recrystallized from a mixed solvent of ethanol and diisopropyl ether to give the desired product (295 mg, 88.5%) as a solid.