Water → HCID 19074340, 화합물

HRID 964935노트

반응식

HRID 964935 반응식
[H-].[H-].[H-].[H-].[Li+].[Al+3].[Cl:7][C:8]1[CH:23]=[CH:22][C:11]2[C:12](=O)[NH:13][C:14]3[CH:20]=[CH:19][CH:18]=[CH:17][C:15]=3[O:16][C:10]=2[CH:9]=1.O>O1CCCC1.O1CCOCC1>[Cl:7][C:8]1[CH:23]=[CH:22][C:11]2[CH2:12][NH:13][C:14]3[CH:20]=[CH:19][CH:18]=[CH:17][C:15]=3[O:16][C:10]=2[CH:9]=1

참가 물질

6

반응물 3

HCID 962WaterHCID 190743493158-88-1HCID 21226445Aluminium lithium hydride

생성물 1

HCID 19074340HCID 19074340, 화합물수율 84%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 312751,4-Dioxane용매

실험 절차

LiAlH4 (1M) in tetrahydrofuran (100 ml) was added dropwise to a mixture of 3-chlorodibenz[b,f][1,4]oxazepin-11(10H)-one (12.3 g) (prepared as described in Indian J. Chem. 1974, 12(3), 227-35) in 1,4-dioxane (400ml) under a N2 atmosphere. The mixture was stirred, refluxed for 1 hour 30 minutes, cooled and water was added dropwise. The mixture was acidified and extracted with EtOAc. The organic layer was dried with Na2SO4, filtered off and evaporated. The residue was purified by open column chromatography over silica gel (eluent: CH2Cl2). The pure fractions were collected and evaporated, yielding 9.74 g (84%) of 3-chloro-10,11-dihydrodibenz[b,f]-[1,4]oxazepine (interm.8).

후처리

  1. temperaturerefluxed for 1 hour 30 minutes
  2. temperaturecooled
  3. extractionextracted with EtOAc
  4. dry with materialThe organic layer was dried with Na2SO4
  5. filtrationfiltered off
  6. customevaporated
  7. customThe residue was purified by open column chromatography over silica gel (eluent: CH2Cl2)
  8. customThe pure fractions were collected
  9. customevaporated

출처 및 근거

ORD 기록
ord-ac3ae8b737ee474e9feeec00caf212b9
출처 데이터셋
uspto-grants-1998_06
특허 번호
US05773433

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