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.FC(F)(F)C(O)=O.C(Cl)Cl>CC(C)=O.C(=O)([O-])[O-].[K+].[K+]>[CH3:26][C:24]1[S:25][C:21]2[CH:20]=[CH:19][C:18]([O:17][CH2:16][CH: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
反応物 2
生成物 1
試薬・触媒・溶媒 2
実験手順
A solution of 4-[2-hydroxy-3-(2-methylbenzothiazol-5-yloxy)propyl]-piperazine-1-carboxylic acid tert-butyl ester, a compound of formula (5) (2.0 g, 4.9 mmol), and 25% trifluoroacetic acid/methylene chloride (20 ml) was allowed to stir at room temperature overnight. The solvent was evaporated (in vacuo) to yield an oil. The oil was diluted with acetone (20 ml) and solid potassium carbonate was added until the foaming stopped. The resulting mixture was allowed to stir overnight. The solution was filtered through Celite 512, and the filtrate was evaporated (in vacuo), to yield an oil. The oil was placed under high vacuum overnight, to yield 1-(2-methylbenzothiazol-5-yloxy)-3-piperazin-1-ylpropan-2-ol, as a clear viscous oil (3.4 g. 6.3 mmol).
後処理
- customThe solvent was evaporated (in vacuo)
- customto yield an oil
- additionwas added until the foaming
- stirringto stir overnight
- filtrationThe solution was filtered through Celite 512
- customthe filtrate was evaporated (in vacuo)
- customto yield an oil
- customwas placed under high vacuum overnight
出典と根拠
- ORDレコード
- ord-d07b9fcd9cd9436785e486ee7507f440
- 出典データセット
- uspto-grants-2005_08
- 特許番号
- US06930111B2
関連ノート
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