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Ammonium Hydroxide → Ammonium Hydroxide

HRID 1246704
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HRID 1246704 반응식
FC(F)(F)C([N:5]1[CH2:11][CH:10]2[N:12]([C:13]([O:15][C:16]([CH3:19])([CH3:18])[CH3:17])=[O:14])[CH:7]([CH2:8][CH2:9]2)[CH2:6]1)=[O:4].[OH-].[NH4+]>CO>[NH4+:5].[OH-:4].[CH:7]12[N:12]([C:13]([O:15][C:16]([CH3:19])([CH3:18])[CH3:17])=[O:14])[CH:10]([CH2:9][CH2:8]1)[CH2:11][NH:5][CH2:6]2
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참가 물질

5

반응물 2

HCID 14923Ammonium HydroxideHCID 21904733tert-Butyl 3-(trifluoroacetyl)-3,8-diazabicyclo[3.2.1]octane-8-carboxylate

생성물 2

HCID 14923Ammonium Hydroxide수율 1%HCID 157409088-Boc-3,8-diaza-bicyclo(3.2.1)octane

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

tert-Butyl 3-(trifluoroacetyl)-3,8-diazabicyclo[3.2.1]octane-8-carboxylate (6.54 mmol) in methanol (85 mL) was treated with ammonium hydroxide (8.5 mL) and stirred overnight at room temperature. The mixture was concentrated under reduced pressure and purified by chromatography on silica gel (5% MeOH, 0.5% NH4OH in CH2Cl2; then 10% MeOH, 1% NH4OH in CH2Cl2) to provide the title compound. MS (DCI/NH3) m/z: 213 (M+H)+; 1H NMR (CDCl3) δ 1.47 (s, 9H), 1.81 (m, 2H), 1.94 (m, 2H), 2.65 (dd, 2H), 3.00 (br, 2H), 4.11 (br, 2H).

후처리

  1. concentrationThe mixture was concentrated under reduced pressure
  2. custompurified by chromatography on silica gel (5% MeOH, 0.5% NH4OH in CH2Cl2

출처 및 근거

ORD 기록
ord-d992aaa1783b43178ac4cb359270d984
출처 데이터셋
uspto-grants-2006_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07129235B2

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