Water → HCID 14809498, 화합물

HRID 649323노트

반응식

HRID 649323 반응식
[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

참가 물질

7

반응물 5

HCID 962WaterHCID 80061-Bromo-3-chloropropaneHCID 8857Ethyl AcetateHCID 24758Sodium hydrideHCID 14809494HCID 14809494, 화합물

생성물 1

HCID 14809498HCID 14809498, 화합물수율 93.4%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c6fcb699b3f44607a6fbae79d18938f3
출처 데이터셋
uspto-grants-1988_04
특허 번호
US04739050

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