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Triethylamine → HCID 50876498、化合物

HRID 901071
ノート
印刷プレビュー

反応式

HRID 901071 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

HCID 50876498HCID 50876498、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-beaaba7b658546198910dcfb0de33e1b
出典データセット
uspto-grants-2008_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07361687B2

反応ノート

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