反応式
C(OC([N:8]1[CH2:13][CH2:12][N:11]([CH2:14][CH:15]([OH:28])[CH2:16][O:17][C:18]2[CH:19]=[CH:20][C:21]3[S:25][C:24]([CH3:26])=[N:23][C:22]=3[CH:27]=2)[CH2:10][CH2:9]1)=O)(C)(C)C>Cl.O1CCOCC1>[CH3:26][C:24]1[S:25][C:21]2[CH:20]=[CH:19][C:18]([O:17][CH2:16][C@H:15]([OH:28])[CH2:14][N:11]3[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]3)=[CH:27][C:22]=2[N:23]=1参加物
実験手順
A solution of 4-[2-hydroxy-3-(2-methylbenzothiazol-5-yloxy)propyl]-piperazine-1-carboxylic acid tert-butyl ester (2.9 g, 7.1 mmol), a compound of formula (5), was dissolved in a 4N solution of HCl in dioxane (20 ml) and allowed to stir at room temperature for 4 hours. The solvent was evaporated under reduced pressure to yield a white solid. The white solid was dried under high vacuum, and then dissolved in methanol (250 ml). AG 1-X8 resin was added and the mixture shaken. Additional resin was added until a neutral pH was obtained. The resin beads were removed by filtration, and methanol removed from the filtrate under reduced pressure, and the residue placed under high vacuum overnight, to yield (2R)-3-(2-methylbenzothiazol-5-yloxy)-1-piperazinylpropan-2-ol as an oil.
後処理
- customThe solvent was evaporated under reduced pressure
- customto yield a white solid
- customThe white solid was dried under high vacuum
- dissolutiondissolved in methanol (250 ml)
- additionAG 1-X8 resin was added
- stirringthe mixture shaken
- additionAdditional resin was added until a neutral pH
- customwas obtained
- customThe resin beads were removed by filtration, and methanol
- customremoved from the filtrate under reduced pressure
- customplaced under high vacuum overnight
出典と根拠
- ORDレコード
- ord-54a443f5f9ce45b4b5b9725e6e3c9f3f
- 出典データセット
- uspto-grants-2007_08
- 特許番号
- US07262198B2
関連ノート
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