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

HRID 246668ノート

反応式

HRID 246668 の反応式
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

参加物

5

反応物 2

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

生成物 1

HCID 71280568Tert-butyl 3-amino-3-methylcyclobutylcarbamate hydrochloride収率 63%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 312751,4-Dioxane溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-e678869c937c4fa4814edcac208e18ae
出典データセット
uspto-grants-2014_02
特許番号
US08658646B2

反応ノート

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