Water → N-(2,4-Dimethoxybenzyl)-C-o-tolylmethanesulfonamide

HRID 339850

反応式

HRID 339850 の反応式
[C:1]1([CH3:12])[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[CH2:7][S:8](Cl)(=[O:10])=[O:9].[CH3:13][O:14][C:15]1[CH:22]=[C:21]([O:23][CH3:24])[CH:20]=[CH:19][C:16]=1[CH2:17][NH2:18].O.C(OCC)(=O)C>ClCCl>[CH3:13][O:14][C:15]1[CH:22]=[C:21]([O:23][CH3:24])[CH:20]=[CH:19][C:16]=1[CH2:17][NH:18][S:8]([CH2:7][C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][C:1]=1[CH3:12])(=[O:10])=[O:9]

参加物

6

反応物 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 5972502,4-DimethoxybenzylamineHCID 2760661(2-methylphenyl)methanesulfonyl Chloride

生成物 1

HCID 68291409N-(2,4-Dimethoxybenzyl)-C-o-tolylmethanesulfonamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

At room temperature, 1.00 g of o-tolylmethanesulfonyl chloride was initially charged in 30 ml of dichloromethane, and 1.46 ml of 2,4-dimethoxybenzylamine were added dropwise. The reaction mixture was stirred for 30 minutes. Then the mixture was admixed with 50 ml of water and 50 ml of ethyl acetate, and then the aqueous phase was washed once more with 30 ml of ethyl acetate. The combined organic phases were washed with 1 N aqueous hydrochloric acid, dried over MgSO4 and concentrated by rotary evaporation. The residue (1.42 g) was used in the next reaction without further purification.

後処理

  1. washthe aqueous phase was washed once more with 30 ml of ethyl acetate
  2. washThe combined organic phases were washed with 1 N aqueous hydrochloric acid
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated by rotary evaporation
  5. customThe residue (1.42 g) was used in the next reaction without further purification

出典と根拠

ORDレコード
ord-bdd0e880a8d546f2bc7409c553806ba2
出典データセット
uspto-grants-2014_11
特許番号
US08895547B2

関連ノート

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