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Methyl [[(methoxycarbonyl)amino](methylthio)methylene]carbamate → HCID 178502035, 화합물

HRID 1823782
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HRID 1823782 반응식
[NH2:1][C:2]1[CH:3]=[C:4]([O:9][S:10]([C:13]2[CH:18]=[CH:17][C:16]([NH:19][CH2:20][CH:21]3[CH2:23][CH2:22]3)=[CH:15][CH:14]=2)(=[O:12])=[O:11])[CH:5]=[CH:6][C:7]=1[NH2:8].[CH3:24][O:25][C:26]([NH:28][C:29](=NC(OC)=O)SC)=[O:27]>C(O)(=O)C.CO>[CH3:24][O:25][C:26]([NH:28][C:29]1[NH:8][C:7]2[CH:6]=[CH:5][C:4]([O:9][S:10]([C:13]3[CH:18]=[CH:17][C:16]([NH:19][CH2:20][CH:21]4[CH2:22][CH2:23]4)=[CH:15][CH:14]=3)(=[O:12])=[O:11])=[CH:3][C:2]=2[N:1]=1)=[O:27]
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참가 물질

5

반응물 2

HCID 98708Methyl [[(methoxycarbonyl)amino](methylthio)methylene]carbamateHCID 865960794-(Cyclopropylmethyl-amino)-benzenesulfonic acid 3,4-diamino-phenyl ester

생성물 1

HCID 178502035HCID 178502035, 화합물수율 46.7%

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 887Methanol용매

실험 절차

To a solution of 4-(cyclopropylmethyl-amino)-benzenesulfonic acid 3,4-diamino-phenyl ester (648 mg) in acetic acid (4.5 ml) and methanol (40 ml) at 80° C. was added 1,3-bis(methoxycarbonyl)-2-methyl-2-thiopseudourea (580 mg). The reaction mixture was refluxed for 4 hours then allowed to cool to ambient temperature and stirred at this temperature for 14 hours. The resultant precipitate was filtered, washed with diethyl ether and dried under vacuum to afford 4-(cyclopropylmethyl-amino)-benzene sulfonic acid 2-methoxycarbonylamino-1H-benzoimidazol-5-yl ester (378 mg) as a beige solid. Mass spectrum: 417 [M+H]+; retention time=13.16 minutes.

후처리

  1. temperatureThe reaction mixture was refluxed for 4 hours
  2. filtrationThe resultant precipitate was filtered
  3. washwashed with diethyl ether
  4. customdried under vacuum

출처 및 근거

ORD 기록
ord-30c39d20c91f45fb8dc98fc8366c8ac4
출처 데이터셋
uspto-grants-2006_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07041668B2

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