Hydrochloric Acid → (S)-2-Amino-N-(3,4-dimethyl-phenyl)-N-[2-(5-methyl-pyridin-2-yl)-ethyl]-2-phenyl-acetamide dihydrochloride

HRID 1094360ノート

反応式

HRID 1094360 の反応式
C(OC(=O)[NH:7][C@H:8]([C:15](=[O:34])[N:16]([C:26]1[CH:31]=[CH:30][C:29]([CH3:32])=[C:28]([CH3:33])[CH:27]=1)[CH2:17][CH2:18][C:19]1[CH:24]=[CH:23][C:22]([CH3:25])=[CH:21][N:20]=1)[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)(C)(C)C.[ClH:36]>O1CCOCC1>[ClH:36].[ClH:36].[NH2:7][C@@H:8]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[C:15]([N:16]([C:26]1[CH:31]=[CH:30][C:29]([CH3:32])=[C:28]([CH3:33])[CH:27]=1)[CH2:17][CH2:18][C:19]1[CH:24]=[CH:23][C:22]([CH3:25])=[CH:21][N:20]=1)=[O:34]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 58007500((S)-{(3,4-dimethyl-phenyl)-[2-(5-methyl-pyridin-2-yl)-ethyl]-carbamoyl}-phenyl-methyl)-carbamic acid tert-butyl ester

生成物 1

HCID 66638324(S)-2-Amino-N-(3,4-dimethyl-phenyl)-N-[2-(5-methyl-pyridin-2-yl)-ethyl]-2-phenyl-acetamide dihydrochloride収率 94%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒2 回

実験手順

To a solution of 50 mg (0.11 mmol) ((S)-{(3,4-dimethyl-phenyl)-[2-(5-methyl-pyridin-2-yl)-ethyl]-carbamoyl}-phenyl-methyl)-carbamic acid tert-butyl ester in 0.2 mL dioxane was added 265 uL (1.06 mmol) of a 4 M HCl solution in dioxane. The mixture was stirred at room temperature for 18 hours. The solvent was removed in vacuo. Ethylacetate was added and the mixture was stirred slowly at ambient temperature. The solid was filtered, rinsed with ether and dried under vacum to provide 0.044 g (94%) of the title compound as a light yellow solid MS (m/e): 374.3 [M+H]+.

後処理

  1. customThe solvent was removed in vacuo
  2. additionEthylacetate was added
  3. stirringthe mixture was stirred slowly at ambient temperature
  4. filtrationThe solid was filtered
  5. washrinsed with ether
  6. customdried under vacum

出典と根拠

ORDレコード
ord-5cca32afd15f4b7782340662653add78
出典データセット
uspto-grants-2012_03
特許番号
US08133909B2

反応ノート

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