HCID 23002992, 화합물 → 7-Chloro-8-morpholin-4-yl-2,3,4,5-tetrahydropyrido[3,2-f][1,4]oxazepine monohydrobromide

HRID 1692607노트

반응식

HRID 1692607 반응식
[Cl:1][C:2]1[C:12]([N:13]2[CH2:18][CH2:17][O:16][CH2:15][CH2:14]2)=[N:11][C:10]2[O:9][CH2:8][CH2:7][N:6](C(OC(C)(C)C)=O)[CH2:5][C:4]=2[CH:3]=1.[BrH:26].C(O)C>C(O)C>[BrH:26].[Cl:1][C:2]1[C:12]([N:13]2[CH2:14][CH2:15][O:16][CH2:17][CH2:18]2)=[N:11][C:10]2[O:9][CH2:8][CH2:7][NH:6][CH2:5][C:4]=2[CH:3]=1

참가 물질

4

반응물 2

HCID 23002992HCID 23002992, 화합물HCID 67279788tert-butyl 7-chloro-8-morpholin-4-yl-2,3-dihydropyrido[3,2-f][1,4]oxazepine-4(5H)-carboxylate

생성물 1

HCID 672802287-Chloro-8-morpholin-4-yl-2,3,4,5-tetrahydropyrido[3,2-f][1,4]oxazepine monohydrobromide수율 25%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of the compound (0.10 g) obtained in step 1 in ethanol (1 mL) was added hydrobromic acid-ethanol solution (1 mL), and the mixture was stirred at room temperature for 4 hr. The solvent was evaporated under reduced pressure, and the aqueous layer was made basic with ethyl acetate and aqueous sodium hydroxide solution. The organic layer was washed with brine and dried, and the solvent was evaporated under reduced pressure. Ethyl acetate was added to the residue, and hydrobromic acid-ethanol solution was added. The precipitate was collected by filtration to give the title compound (0.03 g, 25%) as a white powder.

후처리

  1. customThe solvent was evaporated under reduced pressure
  2. washThe organic layer was washed with brine
  3. customdried
  4. customthe solvent was evaporated under reduced pressure
  5. additionEthyl acetate was added to the residue, and hydrobromic acid-ethanol solution
  6. additionwas added
  7. filtrationThe precipitate was collected by filtration

출처 및 근거

ORD 기록
ord-46e55518a98a4a57b21a3df181202d8b
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08158617B2

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