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Water → methyl 4-((acetylimino)(3-(3-(4-(N-(4-sulfamoylbenzyl)sulfamoyl)phenyl)ureido)phenyl)methyl)piperazine-1-carboxylate

HRID 1797986
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인쇄 미리보기

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HRID 1797986 반응식
[NH:1]=[C:2]([C:13]1[CH:18]=[CH:17][CH:16]=[C:15]([NH:19][C:20]([NH:22][C:23]2[CH:28]=[CH:27][C:26]([S:29](=[O:43])(=[O:42])[NH:30][CH2:31][C:32]3[CH:37]=[CH:36][C:35]([S:38](=[O:41])(=[O:40])[NH2:39])=[CH:34][CH:33]=3)=[CH:25][CH:24]=2)=[O:21])[CH:14]=1)[N:3]1[CH2:8][CH2:7][N:6]([C:9]([O:11][CH3:12])=[O:10])[CH2:5][CH2:4]1.CCN(C(C)C)C(C)C.[C:53](Cl)(=[O:55])[CH3:54].O>C(Cl)Cl.CN(C=O)C>[C:53]([N:1]=[C:2]([C:13]1[CH:18]=[CH:17][CH:16]=[C:15]([NH:19][C:20]([NH:22][C:23]2[CH:24]=[CH:25][C:26]([S:29](=[O:42])(=[O:43])[NH:30][CH2:31][C:32]3[CH:37]=[CH:36][C:35]([S:38](=[O:41])(=[O:40])[NH2:39])=[CH:34][CH:33]=3)=[CH:27][CH:28]=2)=[O:21])[CH:14]=1)[N:3]1[CH2:4][CH2:5][N:6]([C:9]([O:11][CH3:12])=[O:10])[CH2:7][CH2:8]1)(=[O:55])[CH3:54]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 6367Acetyl chlorideHCID 81531DiisopropylethylamineHCID 57496162HCID 57496162, 화합물

생성물 1

HCID 46852302methyl 4-((acetylimino)(3-(3-(4-(N-(4-sulfamoylbenzyl)sulfamoyl)phenyl)ureido)phenyl)methyl)piperazine-1-carboxylate수율 19%

시약·촉매·용매 1

HCID 22350042
dichloromethane N,N-dimethylformamide
용매

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온도
0 °C

실험 절차

100 mg of compound 60 were dissolved in 2 ml of DCM/DMF 1:1 solution, containing 2 eq of DIEA. Under stirring and at 0° C., 6 eq of acetylchloride were added portionwise during 30 minutes. The solution was stirred overnight at rt, then water was added and a precipitate formed. The precipitate was separated and the title compound was obtained after preparative HPLC purification.

후처리

  1. stirringThe solution was stirred overnight at rt
  2. customa precipitate formed
  3. customThe precipitate was separated

출처 및 근거

ORD 기록
ord-8bfd9bf696644d6898cdbc850aa1deaf
출처 데이터셋
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08343963B2

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