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Hydrochloric Acid → Tert-butyl 4-amino-4-methylcyclohexylcarbamate hydrochloride

HRID 246652
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HRID 246652 반응식
CC(C)(S([NH:6][C:7]1([CH3:21])[CH2:12][CH2:11][CH:10]([NH:13][C:14](=[O:20])[O:15][C:16]([CH3:19])([CH3:18])[CH3:17])[CH2:9][CH2:8]1)=O)C.[ClH:23]>CO.O1CCOCC1>[ClH:23].[NH2:6][C:7]1([CH3:21])[CH2:12][CH2:11][CH:10]([NH:13][C:14](=[O:20])[O:15][C:16]([CH3:18])([CH3:17])[CH3:19])[CH2:9][CH2:8]1
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참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 71280131Tert-butyl 4-(1,1-dimethylethylsulfinamido)-4-methylcyclohexylcarbamate

생성물 1

HCID 71279525Tert-butyl 4-amino-4-methylcyclohexylcarbamate hydrochloride수율 63%

시약·촉매·용매 2

HCID 887Methanol용매HCID 312751,4-Dioxane용매

실험 절차

To a stirred solution of tert-butyl 4-(1,1-dimethylethylsulfinamido)-4-methylcyclohexylcarbamate (0.2 g, 0.6 mmol) in 100 mL of MeOH was added a saturated solution of HCl (g) in dioxane (0.72 mL). The solution was stirred at room temperature overnight. The solvent was removed under reduced pressure, the residue was triturated with EtOAc (15 mL), then decanted and dried to give tert-butyl 4-amino-4-methylcyclohexylcarbamate hydrochloride (0.1 g, 63%) as a white solid. MS: (M+H)+=229.2. 1H NMR (300 MHz, CD3OD): δ 3.36 (m, 1H), 1.91-1.66 (m, 9H), 1.40 (s, 9H), 1.18 (s, 3H).

후처리

  1. customThe solvent was removed under reduced pressure
  2. customthe residue was triturated with EtOAc (15 mL)
  3. customdecanted
  4. customdried

출처 및 근거

ORD 기록
ord-aa47209413404b3abcdf0b9f86917b68
출처 데이터셋
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08658646B2

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