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Triethylamine → HCID 50876498, 화합물

HRID 901071
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HRID 901071 반응식
Cl.CN.[Cl:4][C:5]1[C:10]([CH3:11])=[C:9]([Cl:12])[CH:8]=[CH:7][C:6]=1[S:13](Cl)(=[O:15])=[O:14].[CH2:17]([N:19](CC)CC)C>ClCCl>[CH3:17][NH:19][S:13]([C:6]1[CH:7]=[CH:8][C:9]([Cl:12])=[C:10]([CH3:11])[C:5]=1[Cl:4])(=[O:15])=[O:14]
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참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 6364545Methylamine hydrochlorideHCID 157253742,4-Dichloro-3-methylbenzene-1-sulfonyl chloride

생성물 1

HCID 50876498HCID 50876498, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A suspension of 2.55 g (37.8 mM) of methanamine hydrochloride is prepared in 120 ml of dichloromethane (DCM) and 7.5 g of 2,4-dichloro-3-methylbenzenesulphonyl chloride in solution in 30 ml of DCM, and 10.5 ml of triethylamine, are added; the reaction mixture is kept under agitation for 15 hours at ambient temperature and then washed with a solution of 1N hydrochloric acid, with a solution of sodium bicarbonate, and then with water. The organic phase is dried over magnesium sulphate and then concentrated under reduced pressure. The solid residue obtained is purified by chromatography on silica gel in eluting with the aid of a mixture of cyclohexane/ethyl acetate (8/2, v/v). 6.2 g of the expected compound are thus obtained as a white solid (yield=85%).

후처리

  1. washwashed with a solution of 1N hydrochloric acid, with a solution of sodium bicarbonate
  2. dry with materialThe organic phase is dried over magnesium sulphate
  3. concentrationconcentrated under reduced pressure
  4. customThe solid residue obtained
  5. customis purified by chromatography on silica gel
  6. washin eluting with the aid of a mixture of cyclohexane/ethyl acetate (8/2

출처 및 근거

ORD 기록
ord-beaaba7b658546198910dcfb0de33e1b
출처 데이터셋
uspto-grants-2008_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07361687B2

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