Hydrochloric Acid → 7-Bromo-2,3,4,5-tetrahydro-1,4-benzoxazepine hydrochloride

HRID 473848

반응식

HRID 473848 반응식
[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[O:11][CH2:10][CH2:9][N:8](C(OC(C)(C)C)=O)[CH2:7][C:6]=2[CH:19]=1.C(O)C.[ClH:23].O1CCOCC1>C(OCC)C>[ClH:23].[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[O:11][CH2:10][CH2:9][NH:8][CH2:7][C:6]=2[CH:19]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 702EthanolHCID 312751,4-DioxaneHCID 25220760tert-Butyl 7-bromo-2,3-dihydro-1,4-benzoxazepine-4(5H)-carboxylate

생성물 1

HCID 668201377-Bromo-2,3,4,5-tetrahydro-1,4-benzoxazepine hydrochloride수율 98%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

1,1-dimethylethyl 7-bromo-2,3-dihydro-1,4-benzoxazepine-4 (5H)-carboxylate (10 g, 30.5 mmol) was taken into hot ethanol (10 mL) followed by addition of 4M hydrogen chloride in dioxane solution (2.1 eq, 16 mL) and the resulting solution was allowed to slowly cool to ambient temperature over one hour. An excess of ethyl ether was then added and the resulting slurry was filtered. The filter cake was washed with ethyl ether and dried to give 7-bromo-2,3,4,5-tetrahydro-1,4-benzoxazepine hydrochloride (7.9 g, 98% yield) as a colorless crystalline solid. MS (EI) for C9H10NOBr: 229 (MH+).

후처리

  1. filtrationthe resulting slurry was filtered
  2. washThe filter cake was washed with ethyl ether
  3. customdried

출처 및 근거

ORD 기록
ord-3d1c6b8d66da4b39b979a793961ed21b
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08637499B2

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