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Water → 4-(methylthio)-1-tetrahydro-2H-pyran-2-yl-5-(tetrahydro-2H-pyran-2-yloxy)-1H-indazole

HRID 1269925
ノート
印刷プレビュー

反応式

HRID 1269925 の反応式
[CH3:1][S-:2].[Na+].Br[C:5]1[C:13]([O:14][CH:15]2[CH2:20][CH2:19][CH2:18][CH2:17][O:16]2)=[CH:12][CH:11]=[C:10]2[C:6]=1[CH:7]=[N:8][N:9]2[CH:21]1[CH2:26][CH2:25][CH2:24][CH2:23][O:22]1.O>CN(C)C=O>[CH3:1][S:2][C:5]1[C:13]([O:14][CH:15]2[CH2:20][CH2:19][CH2:18][CH2:17][O:16]2)=[CH:12][CH:11]=[C:10]2[C:6]=1[CH:7]=[N:8][N:9]2[CH:21]1[CH2:26][CH2:25][CH2:24][CH2:23][O:22]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 4378561Sodium methanethiolateHCID 694325024-bromo-1-tetrahydro-2H-pyran-2-yl-5-(tetrahydro-2H-pyran-2-yloxy)-1H-indazole

生成物 1

HCID 694312114-(methylthio)-1-tetrahydro-2H-pyran-2-yl-5-(tetrahydro-2H-pyran-2-yloxy)-1H-indazole収率 81.3%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
70 °C

実験手順

Sodium thiomethoxide (0.0265 g, 0.38 mmol) was added to a solution of 4-bromo-1-tetrahydro-2H-pyran-2-yl-5-(tetrahydro-2H-pyran-2-yloxy)-1H-indazole (0.100 g, 0.26 mmol) in N,N-dimethylformamide (1 ml), and the resulting mixture was heated at 70° C. and stirred for 11 hours. The reaction solution was added to water and extracted three times with toluene/ethyl acetate=1/1, and the extract solution was dried over anhydrous magnesium sulfate. The solvent was distilled off and the residue was purified by a silica gel chromatography (hexane/ethyl acetate=10/1) to obtain 4-(methylthio)-1-tetrahydro-2H-pyran-2-yl-5-(tetrahydro-2H-pyran-2-yloxy)-1H-indazole (0.0737 g, 80%).

後処理

  1. extractionextracted three times with toluene/ethyl acetate=1/1
  2. dry with materialthe extract solution was dried over anhydrous magnesium sulfate
  3. distillationThe solvent was distilled off
  4. customthe residue was purified by a silica gel chromatography (hexane/ethyl acetate=10/1)

出典と根拠

ORDレコード
ord-2cebfd3f81ac4c879f1d99e621253371
出典データセット
uspto-grants-2007_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07199147B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート