Water → Methyl 4-(3-chloro-propyl-sulphonyl-amino)-3-methyl-benzoate

HRID 2094269ノート

反応式

HRID 2094269 の反応式
[NH2:1][C:2]1[CH:11]=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[CH:4][C:3]=1[CH3:12].[Cl:13][CH2:14][CH2:15][CH2:16][S:17](Cl)(=[O:19])=[O:18].O.C(OCC)(=O)C>N1C=CC=CC=1>[Cl:13][CH2:14][CH2:15][CH2:16][S:17]([NH:1][C:2]1[CH:11]=[CH:10][C:5]([C:6]([O:8][CH3:9])=[O:7])=[CH:4][C:3]=1[CH3:12])(=[O:19])=[O:18]

参加物

6

反応物 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 154103-Chloropropanesulphonyl chlorideHCID 2736799Methyl 4-amino-3-methylbenzoate

生成物 1

HCID 43654282Methyl 4-(3-chloro-propyl-sulphonyl-amino)-3-methyl-benzoate

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

100 mg (0.61 mmol) methyl 4-amino-3-methyl-benzoate dissolved in 3 ml of pyridine are combined with 82 μl (0.67 mmol) 3-chloropropanesulphonic acid chloride and stirred for 16 hours at ambient temperature. The reaction solution is combined with water and ethyl acetate and then the aqueous phase is again extracted with ethyl acetate. The combined organic phases are dried over sodium sulphate and evaporated down i. vac. The residue is further reacted without any more purification.

後処理

  1. extractionthe aqueous phase is again extracted with ethyl acetate
  2. dry with materialThe combined organic phases are dried over sodium sulphate
  3. customevaporated down i
  4. customThe residue is further reacted without any more purification

出典と根拠

ORDレコード
ord-acf9cc62eec942c88c0f6bf3e0426e6a
出典データセット
uspto-grants-2013_05
特許番号
US08445525B2

反応ノート

読み込み中…