Water → HCID 86621304, 화합물

HRID 914489노트

반응식

HRID 914489 반응식
[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

참가 물질

7

반응물 4

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

생성물 1

HCID 86621304HCID 86621304, 화합물

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-b2b2d4eabd1a4541bbe597fd0f1b47d1
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08026370B2

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