Dichloromethane → 2-nitro-N-(2-pyridin-3-ylethyl)benzenesulfonamide

HRID 68998

反応式

HRID 68998 の反応式
[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[S:10](Cl)(=[O:12])=[O:11])([O-:3])=[O:2].ClCCl.[NH2:17][CH2:18][CH2:19][C:20]1[CH:21]=[N:22][CH:23]=[CH:24][CH:25]=1.C(N(CC)CC)C>O>[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[S:10]([NH:17][CH2:18][CH2:19][C:20]1[CH:21]=[N:22][CH:23]=[CH:24][CH:25]=1)(=[O:12])=[O:11])([O-:3])=[O:2]

参加物

6

反応物 4

HCID 6344DichloromethaneHCID 8471TriethylamineHCID 155402-Nitrobenzenesulfonyl chlorideHCID 8540512-(Pyridin-3-yl)ethan-1-amine

生成物 1

HCID 465565342-nitro-N-(2-pyridin-3-ylethyl)benzenesulfonamide収率 32.9%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

2-Nitrobenzene sulfonyl chloride (11.64 g) was added to a dichloromethane solution (100 ml) of 3-(2-aminoethyl)pyridine (6.11 g) and triethylamine (9 ml) at 0° C. The mixture was stirred at room temperature for 2 hours. Water was added to the reaction mixture, followed by extraction with dichloromethane. The organic layer was dried with anhydrous sodium sulfate, and condensed under reduced pressure. The residue was crystallized from ethyl acetate to give the title compound (5.06 g) as a yellow powder.

後処理

  1. extractionfollowed by extraction with dichloromethane
  2. dry with materialThe organic layer was dried with anhydrous sodium sulfate, and condensed under reduced pressure
  3. customThe residue was crystallized from ethyl acetate

出典と根拠

ORDレコード
ord-c3ccd1da4a8f4ca2bfbf69713a3fb167
出典データセット
uspto-grants-2014_09
特許番号
US08822453B2

関連ノート

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