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4-Toluenesulfonyl chloride → 4-Methoxy-2-p-toluenesulfonyloxymethylpyridine

HRID 1741007
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HRID 1741007 반응식
[OH:1][CH2:2][C:3]1[CH:8]=[C:7]([O:9][CH3:10])[CH:6]=[CH:5][N:4]=1.[C:11]1([CH3:21])[CH:16]=[CH:15][C:14]([S:17](Cl)(=[O:19])=[O:18])=[CH:13][CH:12]=1.C(N(CC)CC)C>C(Cl)Cl>[CH3:10][O:9][C:7]1[CH:6]=[CH:5][N:4]=[C:3]([CH2:2][O:1][S:17]([C:14]2[CH:15]=[CH:16][C:11]([CH3:21])=[CH:12][CH:13]=2)(=[O:19])=[O:18])[CH:8]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 73974-Toluenesulfonyl chlorideHCID 8471TriethylamineHCID 10820596(4-Methoxy-pyridin-2-yl)-methanol

생성물 1

HCID 218343624-Methoxy-2-p-toluenesulfonyloxymethylpyridine수율 103.7%

시약·촉매·용매 1

HCID 6344Dichloromethane용매3회

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온도
0 °C

실험 절차

The 2-hydroxymethyl-4-methoxypyridine, (3.48 g, 0.024 mol) was dissolved in 50 ml CH2Cl2 and cooled to 0° C. The p-toluenesulfonyl chloride (5.7 g, 0.03 mol) was added followed by triethylamine (5 g), in 10 ml of CH2Cl2. After 15 minutes, the reaction was stirred at room temperature for one hour. The reaction was diluted with CH2Cl2 (200 ml) and washed with water. The organic layer was separated and dried with MgSO4, filtered and concentrated to afford 7.3 g of crude subtitle compound suitable for further use.

후처리

  1. washwashed with water
  2. customThe organic layer was separated
  3. dry with materialdried with MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-529afc0034b9436f8c06c3d3605ef849
출처 데이터셋
uspto-grants-1999_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05972972

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