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

HRID 1371452노트

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HRID 1371452 반응식
[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

참가 물질

5

반응물 3

HCID 31297Methanesulfonyl chlorideHCID 81531DiisopropylethylamineHCID 17984664HCID 17984664, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
23 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-de297dd2f4ad40578ef653e040a0dac3
출처 데이터셋
uspto-grants-2007_01
특허 번호
US07157457B2

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