Hydrochloric Acid → Tert-butyl 3-amino-3-methylcyclobutylcarbamate hydrochloride

HRID 246668노트

반응식

HRID 246668 반응식
CC(C)(S([NH:6][C:7]1([CH3:19])[CH2:10][CH:9]([NH:11][C:12](=[O:18])[O:13][C:14]([CH3:17])([CH3:16])[CH3:15])[CH2:8]1)=O)C.[ClH:21]>CO.O1CCOCC1>[ClH:21].[NH2:6][C:7]1([CH3:19])[CH2:10][CH:9]([NH:11][C:12](=[O:18])[O:13][C:14]([CH3:16])([CH3:15])[CH3:17])[CH2:8]1

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 71280661Tert-butyl 3-(1,1-dimethylethylsulfinamido)-3-methylcyclobutylcarbamate

생성물 1

HCID 71280568Tert-butyl 3-amino-3-methylcyclobutylcarbamate hydrochloride수율 63%

시약·촉매·용매 2

HCID 887Methanol용매HCID 312751,4-Dioxane용매

실험 절차

To a stirred solution of tert-butyl 3-(1,1-dimethylethylsulfinamido)-3-methylcyclobutylcarbamate (0.45 g, 1.48 mmol) in 150 mL of MeOH was added 2N HCl in dioxane (1.8 mL). The solution was stirred at room temperature overnight. The solvent was removed under reduced pressure, and the residue was triturated with EtOAc, then decanted and dried to give tert-butyl 3-amino-3-methylcyclobutylcarbamate hydrochloride (0.22 g, 63%) as a white solid. MS: (M+H)+=201.2; 1H NMR (300 MHz, DMSO): δ 2.24-2.22 (m, 1H), 1.43-1.383 (m, 13H), 1.10 (s, 3H).

후처리

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

출처 및 근거

ORD 기록
ord-e678869c937c4fa4814edcac208e18ae
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08658646B2

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