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4-Methyl-6,7-dihydro-5H-cyclopenta[d]pyrimidin-2-amine → HCID 13068372, 화합물

HRID 1759136
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HRID 1759136 반응식
[CH3:1][C:2]1[C:7]2[CH2:8][CH2:9][CH2:10][C:6]=2[N:5]=[C:4]([NH2:11])[N:3]=1.[N+:12]([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[S:21]([N:24]=[C:25]=[O:26])(=[O:23])=[O:22])([O-:14])=[O:13]>C(Cl)Cl>[CH3:1][C:2]1[C:7]2[CH2:8][CH2:9][CH2:10][C:6]=2[N:5]=[C:4]([NH:11][C:25]([NH:24][S:21]([C:16]2[CH:17]=[CH:18][CH:19]=[CH:20][C:15]=2[N+:12]([O-:14])=[O:13])(=[O:22])=[O:23])=[O:26])[N:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 9042124-Methyl-6,7-dihydro-5H-cyclopenta[d]pyrimidin-2-amineHCID 111388842-Nitrobenzenesulfonyl isocyanate

생성물 1

HCID 13068372HCID 13068372, 화합물수율 60.9%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a dry, stirred solution of 10 g of 6,7-dihydro-4-methyl-5H-cyclopentapyrimidin-2-amine in 800 ml of methylene chloride at ambient temperature and pressure was added 14.9 g of 2-nitrobenzenesulfonylisocyanate. The resulting mixture was stirred at reflux temperature (42°) for 2 hours after which the methylene chloride was removed under reduced pressure. The resulting solid was triturated with methanol or 1-chlorobutane and filtered to yield 15 g of N-[(6,7-dihydro-4-methyl-5H-cyclopentapyrimidin-2-yl)aminocarbonyl]-2-nitrobenzene-sulfonamide, m.p. 202°-205°. The product showed characteristic absorption bands in the infrared spectrum at 1675 cm-1 and at 1.7, 3.2 and 7.7 to 8.5 ppms by nuclear magnetic resonance spectrum (60 MHz), indicating the title compound.

후처리

  1. customwas removed under reduced pressure
  2. customThe resulting solid was triturated with methanol or 1-chlorobutane
  3. filtrationfiltered

출처 및 근거

ORD 기록
ord-b13bcfaa47984d9a9ee448544d5c14c7
출처 데이터셋
uspto-grants-1982_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04339267

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