Sodium hydride → 6-(3-Dimethylaminopropyl)-1,9-dimethyl-7,8,9,10-tetrahydrothieno[3,2-e]pyrido[4,3-b]indole dihydrochloride

HRID 647947ノート

反応式

HRID 647947 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][N:16]([CH3:18])[CH2:17][C:8]3=1.[H-].[Na+].[CH3:21][N:22]([CH3:27])[CH2:23][CH2:24][CH2:25][Cl:26]>CN(C)C=O>[ClH:26].[ClH:26].[CH3:21][N:22]([CH3:27])[CH2:23][CH2:24][CH2:25][N:10]1[C:11]2[C:7](=[C:6]3[C:2]([CH3:1])=[CH:3][S:4][C:5]3=[CH:13][CH:12]=2)[C:8]2[CH2:17][N:16]([CH3:18])[CH2:15][CH2:14][C:9]1=2

参加物

5

反応物 3

HCID 24758Sodium hydrideHCID 669603-Chloro-N,N-dimethyl-1-propanamineHCID 71140Tienocarbine

生成物 1

HCID 204843326-(3-Dimethylaminopropyl)-1,9-dimethyl-7,8,9,10-tetrahydrothieno[3,2-e]pyrido[4,3-b]indole dihydrochloride

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

4.0 g of 1,9-dimethyl-7,8,9,10-tetrahydrothieno[3,2-e]pyrido[4,3-b]indole are dissolved in 60 ml of dimethylformamide, 0.78 g of a 50% strength dispersion of NaH is added, whilst stirring, and, after 1 hour, 2.4 g of 3-dimethylaminopropyl chloride are added. After leaving the mixture is stand for 15 hours, the solvent is evaporated off, the residue is taken up in ethyl acetate, the ethyl acetate mixture is washed and dried and the product is purified on SiO2 with chloroform/methanol (1:1). The dihydrochloride is then prepared with isopropyl alcohol/HCl. Melting point: 263° C.

後処理

  1. customAfter leaving the mixture
  2. customfor 15 hours
  3. customthe solvent is evaporated off
  4. washthe ethyl acetate mixture is washed
  5. customdried
  6. customthe product is purified on SiO2 with chloroform/methanol (1:1)
  7. customThe dihydrochloride is then prepared with isopropyl alcohol/HCl

出典と根拠

ORDレコード
ord-955e843a4889417c8d3ad22bb3185a4a
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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