Dichloromethane → 5-amino-7-(methoxyacetyl)-5,7-dihydro-6H-dibenz[b,d]azepin-6-one hydrochloride

HRID 480774ノート

反応式

HRID 480774 の反応式
C([NH:8][N:9]1[C:15](=[O:16])[CH2:14][C:13]2[CH:17]=[CH:18][CH:19]=[CH:20][C:12]=2[C:11]2[CH:21]=[CH:22][CH:23]=[CH:24][C:10]1=2)(OC(C)(C)C)=O.[C:25]([O-:28])([O-])=O.[Cs+].[Cs+].[C:31]([O:34][CH2:35]Br)(=O)C.C(Cl)[Cl:38]>CN(C=O)C>[ClH:38].[NH2:8][N:9]1[C:15](=[O:16])[CH:14]([C:25](=[O:28])[CH2:31][O:34][CH3:35])[C:13]2[CH:17]=[CH:18][CH:19]=[CH:20][C:12]=2[C:11]2[CH:21]=[CH:22][CH:23]=[CH:24][C:10]1=2

参加物

6

反応物 4

HCID 6344DichloromethaneHCID 10796Cesium carbonateHCID 68536Bromomethyl acetateHCID 114935485-(N-Boc-amino)-5,7-dihydro-6H-dibez[b,d]azepin-6-one

生成物 1

HCID 223126355-amino-7-(methoxyacetyl)-5,7-dihydro-6H-dibenz[b,d]azepin-6-one hydrochloride

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
60 °C

実験手順

A solution of 5-(N-Boc-amino)-5,7-dihydro-6H-dibenz[b,d]azepin-6-one (1.03, 3.08 mmol) (Example 7-E) in DMF was treated with Cs2CO3 (1.10 g, 3.39 mmol) and warmed to 60° C. To the reaction mixture was added bromomethyl acetate (0.321 ml, 3.39 mmol) (Aldrich) and stirring continued for 17 h. After cooling to 23° C. the mixture was diluted with CH2Cl2, washed with several portions of brine and dried over Na2SO4. The title compound was purified by chromatography (SiO2, CHCl3).

後処理

  1. temperatureAfter cooling to 23° C. the mixture
  2. washwashed with several portions of brine
  3. dry with materialdried over Na2SO4
  4. customThe title compound was purified by chromatography (SiO2, CHCl3)

出典と根拠

ORDレコード
ord-f53dd6aabbf640279e24bf9b635ffcfa
出典データセット
uspto-grants-2003_11
特許番号
US06653303B1

反応ノート

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