Water → HCID 14809498、化合物

HRID 649323ノート

反応式

HRID 649323 の反応式
[H-].[Na+].Br[CH2:4][CH2:5][CH2:6][Cl:7].C(OCC)(=O)C.O.[OH:15][C:16]1[CH:21]=[CH:20][C:19]([O:22][CH3:23])=[CH:18][C:17]=1[C:24]1([S:36][CH3:37])[C:29](=[O:30])[N:28]([CH3:31])[C:27]2[CH:32]=[CH:33][CH:34]=[CH:35][C:26]=2[S:25]1>CN(C)C=O>[Cl:7][CH2:6][CH2:5][CH2:4][O:15][C:16]1[CH:21]=[CH:20][C:19]([O:22][CH3:23])=[CH:18][C:17]=1[C:24]1([S:36][CH3:37])[C:29](=[O:30])[N:28]([CH3:31])[C:27]2[CH:32]=[CH:33][CH:34]=[CH:35][C:26]=2[S:25]1

参加物

7

反応物 5

HCID 962WaterHCID 80061-Bromo-3-chloropropaneHCID 8857Ethyl AcetateHCID 24758Sodium hydrideHCID 14809494HCID 14809494、化合物

生成物 1

HCID 14809498HCID 14809498、化合物収率 93.4%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

To a stirred suspension of 60% sodium hydride (0.5 g) in dimethylformamide (10 ml), 3,4-dihydro-2-(2-hydroxy-5-methoxyphenyl)-4-methyl-2-methylthio-3-oxo-2H-1,4-benzothiazine (3.5 g, compound No. 8) dissolved in dimethylformamide (5 ml) is added under nitrogen atmosphere and ice-cooling, and the mixture is stirred for 10 minutes at room temperature. 1-Bromo-3-chloropropane (1.9 g) is added to the reaction mixture, and the mixture is stirred for 1 hour at 50°-60° C. The mixture is poured into a mixture of ethyl acetate and water. The organic layer is washed with saturated aqueous sodium chloride solution, dried over anhydrous sodium sulfate and concentrated in vacuo. The separated crystals are collected by filtration to give 4.0 g (93.4%) of the titled compound.

後処理

  1. additionis added under nitrogen atmosphere
  2. temperatureice-cooling
  3. stirringthe mixture is stirred for 1 hour at 50°-60° C
  4. washThe organic layer is washed with saturated aqueous sodium chloride solution
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated in vacuo
  7. filtrationThe separated crystals are collected by filtration

出典と根拠

ORDレコード
ord-c6fcb699b3f44607a6fbae79d18938f3
出典データセット
uspto-grants-1988_04
特許番号
US04739050

反応ノート

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