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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Methanol → Carbamic acid, N-(4-amino-1-methylcyclohexyl)-, 1,1-dimethylethyl ester

HRID 869243
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HRID 869243 반응식
[CH3:1][C:2]1([NH:9][C:10](=[O:16])[O:11][C:12]([CH3:15])([CH3:14])[CH3:13])[CH2:7][CH2:6][C:5](=O)[CH2:4][CH2:3]1.CO.C([O-])=O.[NH4+:22]>[Pd].O>[NH2:22][CH:5]1[CH2:6][CH2:7][C:2]([NH:9][C:10](=[O:16])[O:11][C:12]([CH3:15])([CH3:14])[CH3:13])([CH3:1])[CH2:3][CH2:4]1
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참가 물질

6

반응물 3

HCID 887MethanolHCID 2723923Ammonium formateHCID 21882608tert-butyl N-(1-methyl-4-oxocyclohexyl)carbamate

생성물 1

HCID 20754832Carbamic acid, N-(4-amino-1-methylcyclohexyl)-, 1,1-dimethylethyl ester수율 92.8%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 962
Water
용매

실험 절차

To a mixture of tert-butyl (1-methyl-4-oxocyclohexyl)carbamate (4.00 g) and methanol (50 mL), ammonium formate (10.2 g) and water (5 mL) were added and stirred for 1 hour until they were completely dissolved. Then, 10% palladium on carbon (2.0 g) was added and stirred at room temperature for 65 hours. After insoluble materials were separated by filtration through celite, the solvent was distilled off, and chloroform was added to the resulting residue, followed by drying over anhydrous magnesium sulfate. The solvent was distilled off to give tert-butyl (4-amino-1-methylcyclohexyl)carbamate (3.73 g) as a colorless syrup.

후처리

  1. additionwere added
  2. dissolutionwere completely dissolved
  3. stirringstirred at room temperature for 65 hours
  4. customAfter insoluble materials were separated by filtration through celite
  5. distillationthe solvent was distilled off
  6. additionchloroform was added to the resulting residue
  7. dry with materialby drying over anhydrous magnesium sulfate
  8. distillationThe solvent was distilled off

출처 및 근거

ORD 기록
ord-2cbd4b36e7ae45179ab9477a99b5524e
출처 데이터셋
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08969336B2

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