Dimethylformamide → Ethyl trans-5-(4-ethoxy-2-methoxyphenyl)-7-chloro-1-neopentyl-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-acetate

HRID 1811

反応式

HRID 1811 の反応式
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]([CH2:12][C:13]([CH3:16])([CH3:15])[CH3:14])[C:10](=[O:17])[C@@H:9]([CH2:18][C:19]([O:21][CH2:22][CH3:23])=[O:20])[O:8][C@H:7]([C:24]3[CH:29]=[CH:28][C:27]([OH:30])=[CH:26][C:25]=3[O:31][CH3:32])[C:6]=2[CH:33]=1.[CH2:34](I)[CH3:35].C(=O)([O-])[O-].[K+].[K+].CN(C)C=O>O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]([CH2:12][C:13]([CH3:15])([CH3:14])[CH3:16])[C:10](=[O:17])[C@@H:9]([CH2:18][C:19]([O:21][CH2:22][CH3:23])=[O:20])[O:8][C@H:7]([C:24]3[CH:29]=[CH:28][C:27]([O:30][CH2:34][CH3:35])=[CH:26][C:25]=3[O:31][CH3:32])[C:6]=2[CH:33]=1

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 6340IodoethaneHCID 11430Potassium CarbonateHCID 67603286Ethyl trans-7-chloro-5-(4-hydroxy-2-methoxyphenyl)-1-neopentyl-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-acetate

生成物 1

HCID 67603127Ethyl trans-5-(4-ethoxy-2-methoxyphenyl)-7-chloro-1-neopentyl-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-acetate

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of ethyl trans-7-chloro-5-(4-hydroxy-2-methoxyphenyl)-1-neopentyl-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-acetate (0.25 g), ethyl iodide (0.06 ml), potassium carbonate (0.15 g) and N,N-dimethylformamide (200 ml) was stirred for 3 h. The mixture was diluted with water (50 ml) and extracted with ethyl acetate (100 ml). The extract was washed with 1N hydrochloric acid and aqueous sodium bicarbonate, dried over magnesium sulfate and concentrated in vacuo to give ethyl trans-7-chloro-5-(4-ethoxy-2-methoxyphenyl)-1-neopentyl-2-oxo-1,2,3,5-tetrahydro-4,1-benzoxazepine-3-acetate (0.24 g) as colorless crystals (mp=164°-166° C.).

後処理

  1. extractionextracted with ethyl acetate (100 ml)
  2. washThe extract was washed with 1N hydrochloric acid and aqueous sodium bicarbonate
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-077138807f014cf5b7519e136115f695
出典データセット
uspto-grants-1998_03
特許番号
US05726306

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