Methanesulfonyl chloride → N-{[4-(3,4-dichlorobenzyl)morpholin-2-yl]methyl}-N'-[1-(methylsulfonyl)piperidin-4-yl]urea

HRID 1371452ノート

反応式

HRID 1371452 の反応式
[CH3:1][S:2](Cl)(=[O:4])=[O:3].Cl.[Cl:7][C:8]1[CH:9]=[C:10]([CH:29]=[CH:30][C:31]=1[Cl:32])[CH2:11][N:12]1[CH2:17][CH2:16][O:15][CH:14]([CH2:18][NH:19][C:20]([NH:22][CH:23]2[CH2:28][CH2:27][NH:26][CH2:25][CH2:24]2)=[O:21])[CH2:13]1.C(N(CC)C(C)C)(C)C>ClCCl>[Cl:7][C:8]1[CH:9]=[C:10]([CH:29]=[CH:30][C:31]=1[Cl:32])[CH2:11][N:12]1[CH2:17][CH2:16][O:15][CH:14]([CH2:18][NH:19][C:20]([NH:22][CH:23]2[CH2:24][CH2:25][N:26]([S:2]([CH3:1])(=[O:4])=[O:3])[CH2:27][CH2:28]2)=[O:21])[CH2:13]1

参加物

5

反応物 3

HCID 31297Methanesulfonyl chlorideHCID 81531DiisopropylethylamineHCID 17984664HCID 17984664、化合物

生成物 1

HCID 17984682N-{[4-(3,4-dichlorobenzyl)morpholin-2-yl]methyl}-N'-[1-(methylsulfonyl)piperidin-4-yl]urea

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
23 °C

実験手順

Methane sulphonyl chloride (0.009 ml) was added to a solution of Intermediate 16 (0.04 g) and N,N-diisopropylethylamine (0.048 ml) in dichloromethane (3 ml). The solution was stirred for 5 h at 23° C. The solvent was removed in vacuo and the residue was purified by solid phase extraction (Isolute SCX sulphonic acid column) eluting with methanol followed by 10% 0.880 ammonia solution in methanol, to give the title compound as a pale yellow gum (0.034 g).

後処理

  1. customThe solvent was removed in vacuo
  2. customthe residue was purified by solid phase extraction (Isolute SCX sulphonic acid column)
  3. washeluting with methanol

出典と根拠

ORDレコード
ord-de297dd2f4ad40578ef653e040a0dac3
出典データセット
uspto-grants-2007_01
特許番号
US07157457B2

反応ノート

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