Water → HCID 18670322、化合物

HRID 1059406

反応式

HRID 1059406 の反応式
[CH3:1][O:2][CH2:3][N:4]1[C:9]2[CH:10]=[C:11]([C:14]([C:17]3[CH:18]=[N:19][CH:20]=[CH:21][CH:22]=3)(O)[CH3:15])[CH:12]=[CH:13][C:8]=2[S:7][C:6]2[N:23]=[CH:24][CH:25]=[N:26][C:5]1=2.ClS(OC)(=O)=O.O.C(OCC)(=O)C>ClCCl>[N:19]1[CH:20]=[CH:21][CH:22]=[C:17]([C:14]([C:11]2[CH:12]=[CH:13][C:8]3[S:7][C:6]4[N:23]=[CH:24][CH:25]=[N:26][C:5]=4[N:4]([CH2:3][O:2][CH3:1])[C:9]=3[CH:10]=2)=[CH2:15])[CH:18]=1

参加物

6

反応物 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 69938Methyl chlorosulphateHCID 18670441HCID 18670441、化合物

生成物 1

HCID 18670322HCID 18670322、化合物収率 79.8%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 303 mg of 1-(10-methoxymethyl-10H-pyrazino[2,3-b][1,4]benzothiazin-8-yl)1-(pyridin-3-yl)ethanol in dichloromethane was added in a nitrogen atmosphere 0.32 ml of methyl chlorosulfonate and the resulting mixture was heated under reflux for 2 hours. Then the reaction mixture was brought back to room temperature and distributed into water and ethyl acetate. The extract was dried over anhydrous magnesium sulfate and filtered. After distilling off the solvent under reduced pressure, the residue was purified by silica gel column chromatography (eluted with dichloromethane/methanol) to thereby give 230 mg of the title compound as a yellow solid.

後処理

  1. temperaturethe resulting mixture was heated
  2. temperatureunder reflux for 2 hours
  3. customwas brought back to room temperature
  4. dry with materialThe extract was dried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. distillationAfter distilling off the solvent under reduced pressure
  7. customthe residue was purified by silica gel column chromatography (eluted with dichloromethane/methanol)

出典と根拠

ORDレコード
ord-03dc200643aa4ec2bda2b17c98c9faf0
出典データセット
uspto-grants-2003_02
特許番号
US06518423B1

関連ノート

読み込み中…