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

HRID 1371456
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HRID 1371456 반응식
[CH3:1][S:2](Cl)(=[O:4])=[O:3].Cl.Cl.[Cl:8][C:9]1[CH:10]=[C:11]([CH:31]=[CH:32][C:33]=1[Cl:34])[CH2:12][N:13]1[CH2:18][CH2:17][O:16][C@@H:15]([CH2:19][NH:20][C:21]([NH:23][CH2:24][CH:25]2[CH2:30][CH2:29][NH:28][CH2:27][CH2:26]2)=[O:22])[CH2:14]1.C(N(CC)C(C)C)(C)C>ClCCl>[Cl:8][C:9]1[CH:10]=[C:11]([CH:31]=[CH:32][C:33]=1[Cl:34])[CH2:12][N:13]1[CH2:18][CH2:17][O:16][C@@H:15]([CH2:19][NH:20][C:21]([NH:23][CH2:24][CH:25]2[CH2:30][CH2:29][N:28]([S:2]([CH3:1])(=[O:4])=[O:3])[CH2:27][CH2:26]2)=[O:22])[CH2:14]1
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참가 물질

5

반응물 3

HCID 31297Methanesulfonyl chlorideHCID 81531DiisopropylethylamineHCID 69507286HCID 69507286, 화합물

생성물 1

HCID 69507201n-{[(2s)-4-(3,4-Dichlorobenzyl)morpholin-2-yl]methyl}-n'-{[1-(methylsulfonyl)piperidin-4-yl]methyl}urea

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
23 °C

실험 절차

Methane sulphonyl choride (0.013 ml) was added to a solution of Intermediate 18 (0.054 g) and N,N-diisopropylethylamine (0.063 ml) in dichloromethane (2 ml). The solution was stirred for 16 h at 23° C. The solvent was removed in vacuo and the residue 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 clear gum (0.035 g).

후처리

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

출처 및 근거

ORD 기록
ord-0c256e7cbc6844368cb96c9e2f7c8605
출처 데이터셋
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07157457B2

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