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Sodium Carbonate → N-[(1-ethyl-2-pyrrolidinyl)methyl]-4-(7-trifluoromethyl-4-quinazolinylamino)benzamide

HRID 570064
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HRID 570064 반응식
[NH2:1][CH2:2][CH:3]1[CH2:7][CH2:6][CH2:5][N:4]1[CH2:8][CH3:9].[C:10](=[O:13])([O-])[O-].[Na+].[Na+].Cl.[F:17][C:18]([F:41])([F:40])[C:19]1[CH:28]=[C:27]2[C:22]([C:23]([NH:29][C:30]3[CH:35]=[CH:34][C:33](S(Cl)(=O)=O)=[CH:32][CH:31]=3)=[N:24][CH:25]=[N:26]2)=[CH:21][CH:20]=1>C(Cl)(Cl)Cl>[CH2:8]([N:4]1[CH2:5][CH2:6][CH2:7][CH:3]1[CH2:2][NH:1][C:10](=[O:13])[C:33]1[CH:32]=[CH:31][C:30]([NH:29][C:23]2[C:22]3[C:27](=[CH:28][C:19]([C:18]([F:40])([F:41])[F:17])=[CH:20][CH:21]=3)[N:26]=[CH:25][N:24]=2)=[CH:35][CH:34]=1)[CH3:9]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 10340Sodium CarbonateHCID 1172952-Aminomethyl-1-ethylpyrrolidineHCID 867412594-(7-Trifluoromethyl-4-quinazolinylamino)benzene sulphonylchloride hydrochloride

생성물 1

HCID 21273959N-[(1-ethyl-2-pyrrolidinyl)methyl]-4-(7-trifluoromethyl-4-quinazolinylamino)benzamide수율 26.9%

시약·촉매·용매 1

HCID 6212Chloroform
용매

실험 절차

A mixture of 2-aminomethyl-1-ethylpyrrolidine (0.34 ml; 0.00235 mole), anhydrous sodium carbonate (3.5 g) and chloroform (100 ml) was cooled on an ice bath and treated with 4-(7-trifluoromethyl-4-quinazolinylamino) benzene sulphonylchloride hydrochloride (1.0 g; 0.00235 mole) with vigorous stirring. The mixture was stirred at ambient temperature for 4 hours and then filtered. The residue on evaporation of the solvent was triturated with ether and the resulting solid was filtered off, washed with a little ether and dried to give the one-fourth hydrate of the title compound (0.28 g), melting point 150°-152° C.

후처리

  1. temperaturewas cooled on an ice bath
  2. filtrationfiltered
  3. customThe residue on evaporation of the solvent
  4. customwas triturated with ether
  5. filtrationthe resulting solid was filtered off
  6. washwashed with a little ether
  7. customdried

출처 및 근거

ORD 기록
ord-2125172c98c5459c9bed204310ad8ca5
출처 데이터셋
uspto-grants-1988_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04734510

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