Water → HCID 86621304、化合物

HRID 914489ノート

反応式

HRID 914489 の反応式
[CH:1]1([O:7][CH2:8][CH2:9][CH2:10]O)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.C(N(CC)CC)C.[C:19]1([CH3:29])[CH:24]=[CH:23][C:22]([S:25](Cl)(=[O:27])=[O:26])=[CH:21][CH:20]=1.[OH2:30]>ClCCl.CN(C)C1C=CN=CC=1>[CH:1]1([O:7][CH2:8][CH2:9][CH2:10][C:23]2[CH:24]=[C:19]([CH3:29])[CH:20]=[CH:21][C:22]=2[S:25]([OH:30])(=[O:27])=[O:26])[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

参加物

7

反応物 4

HCID 962WaterHCID 73974-Toluenesulfonyl chlorideHCID 8471TriethylamineHCID 100348783-(Cyclohexyloxy)propan-1-ol

生成物 1

HCID 86621304HCID 86621304、化合物

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 6344Dichloromethane溶媒

実験手順

3-(Cyclohexyloxy)propan-1-ol (820 mg) synthesized in Reference Example 47 was dissolved in dichloromethane (20 mL), triethylamine (1.1 mL), p-toluenesulfonyl chloride (1.2 g) and 4-dimethylaminopyridine (63 mg) were added thereto, and the mixture was stirred at room temperature overnight. Water was added to the reaction solution, and the organic layer was separated and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel chromatography (elution solvent; hexane:ethyl acetate=5:1) to give the title compound (1.0 g) as a colorless oil.

後処理

  1. customthe organic layer was separated
  2. dry with materialdried over anhydrous sodium sulfate
  3. customThe solvent was evaporated under reduced pressure
  4. customthe residue was purified by silica gel chromatography (elution solvent; hexane:ethyl acetate=5:1)

出典と根拠

ORDレコード
ord-b2b2d4eabd1a4541bbe597fd0f1b47d1
出典データセット
uspto-grants-2011_09
特許番号
US08026370B2

反応ノート

読み込み中…