Hydrogen chloride-ethyl acetate → 8-(1,2-Dimethylpropoxy)-2,3,4,5-tetrahydropyrido[3,2-f][1,4]oxazepine hydrochloride

HRID 2191257

반응식

HRID 2191257 반응식
[CH3:1][CH:2]([O:6][C:7]1[CH:8]=[CH:9][C:10]2[CH2:11][N:12](C(OC(C)(C)C)=O)[CH2:13][CH2:14][O:15][C:16]=2[N:17]=1)[CH:3]([CH3:5])[CH3:4].[ClH:25].C(OCC)(=O)C>>[ClH:25].[CH3:1][CH:2]([O:6][C:7]1[CH:8]=[CH:9][C:10]2[CH2:11][NH:12][CH2:13][CH2:14][O:15][C:16]=2[N:17]=1)[CH:3]([CH3:4])[CH3:5]

참가 물질

3

반응물 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 68427435tert-butyl 8-(1,2-dimethylpropoxy)-2,3-dihydropyrido[3,2-f][1,4]oxazepine-4(5H)-carboxylate

생성물 1

HCID 684303368-(1,2-Dimethylpropoxy)-2,3,4,5-tetrahydropyrido[3,2-f][1,4]oxazepine hydrochloride수율 52%

실험 절차

A mixture of the compound obtained in step 1 (0.36 g) and 4N hydrogen chloride/ethyl acetate (10 mL) was stirred at room temperature for 3 hr. The precipitate was collected by filtration, and the aqueous layer was basified and extracted with ethyl acetate and aqueous sodium hydroxide solution. The organic layer was washed with saturated brine and dried, and the solvent was evaporated under reduced pressure. Ethyl acetate was added to the residue, and 4N hydrogen chloride/ethyl acetate was added. The precipitate was collected by filtration and recrystallized from ethanol-diisopropyl ether to give the title compound (0.15 g, 52%) as a white powder.

후처리

  1. filtrationThe precipitate was collected by filtration
  2. extractionextracted with ethyl acetate and aqueous sodium hydroxide solution
  3. washThe organic layer was washed with saturated brine
  4. customdried
  5. customthe solvent was evaporated under reduced pressure
  6. additionEthyl acetate was added to the residue, and 4N hydrogen chloride/ethyl acetate
  7. additionwas added
  8. filtrationThe precipitate was collected by filtration
  9. customrecrystallized from ethanol-diisopropyl ether

출처 및 근거

ORD 기록
ord-2a070a86010246e1b5d44d08b45a8049
출처 데이터셋
uspto-grants-2012_12
특허 번호
US08329687B2

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