Ethanol hydrochloride → N-{[(6S,7R)-7-(4-chloro-3-fluorophenyl)-1,4-oxazepan-6-yl]methyl}-2-methoxyacetamide monohydrochloride

HRID 1022627

反応式

HRID 1022627 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C@@H:8]2[O:14][CH2:13][CH2:12][N:11](C(OC(C)(C)C)=O)[CH2:10][C@H:9]2[CH2:22][NH:23][C:24](=[O:28])[CH2:25][O:26][CH3:27])=[CH:4][C:3]=1[F:29].Cl.C(O)C>C(O)C>[ClH:1].[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C@@H:8]2[O:14][CH2:13][CH2:12][NH:11][CH2:10][C@H:9]2[CH2:22][NH:23][C:24](=[O:28])[CH2:25][O:26][CH3:27])=[CH:4][C:3]=1[F:29]

参加物

4

反応物 2

HCID 21887872Ethanol hydrochlorideHCID 66975283tert-butyl (6R,7R)-7-(4-chloro-3-fluorophenyl)-6-{[(methoxyacetyl)amino]methyl}-1,4-oxazepane-4-carboxylate

生成物 1

HCID 66975427N-{[(6S,7R)-7-(4-chloro-3-fluorophenyl)-1,4-oxazepan-6-yl]methyl}-2-methoxyacetamide monohydrochloride収率 151.2%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of tert-butyl (6R,7R)-7-(4-chloro-3-fluorophenyl)-6-{[(methoxyacetyl)amino]methyl}-1,4-oxazepane-4-carboxylate (1.11 g) in ethanol (13 mL) was added 14.0 M hydrogen chloride-ethanol solution (12.0 ml), and the mixture was stirred at room temperature for 1 hr. The crystals obtained by concentration under reduced pressure were recrystallized from ethanol-hexane to give the title compound (715 mg).

後処理

  1. customThe crystals obtained by concentration under reduced pressure
  2. customwere recrystallized from ethanol-hexane

出典と根拠

ORDレコード
ord-aacf8f20d29146ce8ea5aac41f771ec0
出典データセット
uspto-grants-2014_05
特許番号
US08722662B2

関連ノート

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