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Sodium Hydroxide → tert-Butyl 1-methyl-1,3,4,8-tetrahydro-2H-[1,4]oxazepino[6,7-e]indole-2-carboxylate

HRID 2423200
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HRID 2423200 반응식
[CH3:1][CH:2]1[C:8]2=[C:9]3[C:13](=[CH:14][CH:15]=[C:7]2[O:6][CH2:5][CH2:4][N:3]1[C:25]([O:27][C:28]([CH3:31])([CH3:30])[CH3:29])=[O:26])[N:12](S(C1C=CC=CC=1)(=O)=O)[CH:11]=[CH:10]3.[OH-].[Na+]>CCO>[CH3:1][CH:2]1[C:8]2=[C:9]3[C:13](=[CH:14][CH:15]=[C:7]2[O:6][CH2:5][CH2:4][N:3]1[C:25]([O:27][C:28]([CH3:29])([CH3:31])[CH3:30])=[O:26])[NH:12][CH:11]=[CH:10]3
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4

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HCID 14798Sodium HydroxideHCID 67240988tert-Butyl 1-methyl-8-(phenylsulfonyl)-1,3,4,8-tetrahydro-2H-[1,4]oxazepino[6,7-e]indole-2-carboxylate2회

생성물 1

HCID 67242740tert-Butyl 1-methyl-1,3,4,8-tetrahydro-2H-[1,4]oxazepino[6,7-e]indole-2-carboxylate수율 95.3%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
70 °C

실험 절차

To tert-butyl 1-methyl-8-(phenylsulfonyl)-1,3,4,8-tetrahydro-2H-[1,4]oxazepino[6,7-e]indole-2-carboxylate (Intermediate 41, 1.5 g, 3.4 mmol) dissolved in EtOH (50 mL), 2 M NaOH (10 mL, 20 mmol) was added and the reaction mixture was heated at 70° C. for 2 hours. The EtOH was removed under reduced pressure and the water phase was extracted with DCM (2×100 mL). The organic layer was collected, dried (MgSO4) and evaporated to afford the title compound (0.98 g) as a yellow solid. MS m/z 303 [M+H]+.

후처리

  1. customThe EtOH was removed under reduced pressure
  2. extractionthe water phase was extracted with DCM (2×100 mL)
  3. customThe organic layer was collected
  4. dry with materialdried (MgSO4)
  5. customevaporated

출처 및 근거

ORD 기록
ord-25eb8c9d111e4340b0b1cd7b44871194
출처 데이터셋
uspto-grants-2011_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07960374B2

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