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Triethylamine → 2-(Methanesulfonyloxymethyl)-6-methyl-nitrobenzene

HRID 1069476
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반응식

HRID 1069476 반응식
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[CH3:6][C:7]1[C:8]([N+:15]([O-:17])=[O:16])=[C:9]([CH:12]=[CH:13][CH:14]=1)[CH2:10][OH:11].C(N(CC)CC)C>C(Cl)Cl>[CH3:1][S:2]([O:11][CH2:10][C:9]1[CH:12]=[CH:13][CH:14]=[C:7]([CH3:6])[C:8]=1[N+:15]([O-:17])=[O:16])(=[O:4])=[O:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 5619893-Methyl-2-nitrobenzenemethanol

생성물 1

HCID 157669562-(Methanesulfonyloxymethyl)-6-methyl-nitrobenzene수율 97.9%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

At 10-15° C., 27 g (0.23 mol) of methanesulfonyl chloride dissolved in 20 ml of CH2Cl2 is dripped into a mixture of 34 g (0.2 mol) of 3-methyl-2-nitrobenzyl alcohol and 27 g (0.27 mol) of triethylamine in 100 ml of CH2Cl2. The reaction mixture is stirred for 1 hour at room temperature and is then extracted with water. The organic phase is dried over MgSO4 and evaporated down. There is obtained as residue 48 g of the title compound as a yellow oil, containing about 10% of the corresponding benzyl chloride as impurity. The crude product is used for the next reaction without any further purification.

후처리

  1. extractionis then extracted with water
  2. dry with materialThe organic phase is dried over MgSO4
  3. customevaporated down

출처 및 근거

ORD 기록
ord-10634ab235344e1d8cb90a9a5c93b753
출처 데이터셋
uspto-grants-2001_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06252083B1

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