3-Chloro-N,N-dimethyl-1-propanamine → 9-(3-Dimethylaminopropyl)-1-methyl-7,8,9,10-tetrahydrothieno[3,2-e]pyrido[4,3-b]indole

HRID 647944ノート

反応式

HRID 647944 の反応式
[CH3:1][C:2]1[C:6]2=[C:7]3[C:11](=[CH:12][CH:13]=[C:5]2[S:4][CH:3]=1)[NH:10][C:9]1[CH2:14][CH2:15][NH:16][CH2:17][C:8]3=1.[CH3:18][N:19]([CH3:24])[CH2:20][CH2:21][CH2:22]Cl>CN(C)C=O>[CH3:18][N:19]([CH3:24])[CH2:20][CH2:21][CH2:22][N:16]1[CH2:15][CH2:14][C:9]2[NH:10][C:11]3[C:7]([C:8]=2[CH2:17]1)=[C:6]1[C:2]([CH3:1])=[CH:3][S:4][C:5]1=[CH:13][CH:12]=3

参加物

4

反応物 2

HCID 669603-Chloro-N,N-dimethyl-1-propanamineHCID 20484283HCID 20484283、化合物

生成物 1

HCID 204843129-(3-Dimethylaminopropyl)-1-methyl-7,8,9,10-tetrahydrothieno[3,2-e]pyrido[4,3-b]indole

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

10 g of 1-methyl-7,8,9,10-tetrahydrothieno[3,2-e]pyrido[4,3-b]indole, dissolved in 200 ml of dimethylformamide at 90° C., are heated to 90° with a solution of 12 ml of 3-dimethylaminopropyl chloride in 50 ml of dimethylformamide for 3 hours. The reaction mixture is filtered, the filtrate is evaporated and the residue is taken up in chloroform. After washing with water and drying, the organic phase is concentrated, the residue is chromatographed on SiO2 with chloroform/methanol/NH4OH (7:3:0:1) and the product is recrystallised from isopropanol. Melting point: 184° C.

後処理

  1. filtrationThe reaction mixture is filtered
  2. customthe filtrate is evaporated
  3. washAfter washing with water
  4. customdrying
  5. concentrationthe organic phase is concentrated
  6. customthe residue is chromatographed on SiO2 with chloroform/methanol/NH4OH (7:3:0:1)
  7. customthe product is recrystallised from isopropanol

出典と根拠

ORDレコード
ord-623cd7677ddf4e8fb8633c361bf4b97d
出典データセット
uspto-grants-1983_10
特許番号
US04410536

反応ノート

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