Ethanol → HCID 67897170、化合物

HRID 236255

反応式

HRID 236255 の反応式
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

参加物

6

反応物 4

HCID 702EthanolHCID 3776IsopropanolHCID 220210672-Amino-1-(3-bromophenyl)ethan-1-olHCID 67897320HCID 67897320、化合物

生成物 1

HCID 67897170HCID 67897170、化合物収率 65%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-5e9ed521badf4e26ab7ffa2e08247a02
出典データセット
uspto-grants-1987_02
特許番号
US04643849

関連ノート

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