Ethanol → HCID 67897170, 화합물

HRID 236255

반응식

HRID 236255 반응식
C(O)C.[CH3:4][N:5]([CH2:7][C:8]1[S:12][C:11]([CH2:13][S:14][CH2:15][CH2:16][NH:17][C:18](SC)=[CH:19][N+:20]([O-:22])=[O:21])=[CH:10][C:9]=1[CH3:25])[CH3:6].[Br:26][C:27]1[CH:28]=[C:29]([CH:33]([OH:36])[CH2:34][NH2:35])[CH:30]=[CH:31][CH:32]=1.C(O)(C)C>C(OCC)C>[Br:26][C:27]1[CH:28]=[C:29]([CH:33]([OH:36])[CH2:34][NH:35][C:18]([NH:17][CH2:16][CH2:15][S:14][CH2:13][C:11]2[S:12][C:8]([CH2:7][N:5]([CH3:4])[CH3:6])=[C:9]([CH3:25])[CH:10]=2)=[CH:19][N+:20]([O-:22])=[O:21])[CH:30]=[CH:31][CH:32]=1

참가 물질

6

반응물 4

HCID 702EthanolHCID 3776IsopropanolHCID 220210672-Amino-1-(3-bromophenyl)ethan-1-olHCID 67897320HCID 67897320, 화합물

생성물 1

HCID 67897170HCID 67897170, 화합물수율 65%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

With 7.5 ml of ethanol were mixed 4.5 g of 1-{2-[[5-(dimethylamino)methyl-4-methyl-2-thienyl]methylthio]ethylamino}-1-methylthio-2-nitroethene and 3.5 g of DL-[2-(3-bromophenyl)-2-hydroxyethyl]amine, and the resulting mixture was subjected to reaction at room temperature for 30 hours. Thereto were added 5 ml of isopropanol and 30 ml of diethyl ether, and the mixture thus obtained was stirred, after which the crystals formed were collected by filtration. The crystals were recrystallized from 40 ml of isopropanol to obtain 4.3 g (yield 65%) of N-[2-(3-bromophenyl)-2-hydroxyethyl]-N'-{2-[[5-(dimethylamino)methyl-4-methyl-2-thienyl]methylthio]ethyl}-2-nitro-1,1-ethenediamine having a melting point of 104°-106° C.

후처리

  1. customthe resulting mixture was subjected to reaction at room temperature for 30 hours
  2. customthe mixture thus obtained
  3. customafter which the crystals formed
  4. filtrationwere collected by filtration
  5. customThe crystals were recrystallized from 40 ml of isopropanol

출처 및 근거

ORD 기록
ord-5e9ed521badf4e26ab7ffa2e08247a02
출처 데이터셋
uspto-grants-1987_02
특허 번호
US04643849

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