Dipropylamine → 2,6-Bis-(di-n-propylamino-acetylamino)-benzo[1,2-d:5,4-d']bisthiazole dihydrochloride

HRID 67107

反応式

HRID 67107 の反応式
[Cl:1][CH2:2][C:3]([NH:5][C:6]1[S:7][C:8]2[C:9](=[CH:11][C:12]3[N:13]=[C:14]([NH:18][C:19](=[O:22])[CH2:20]Cl)[S:15][C:16]=3[CH:17]=2)[N:10]=1)=[O:4].[CH2:23]([NH:26][CH2:27][CH2:28][CH3:29])[CH2:24][CH3:25]>O1CCOCC1>[ClH:1].[ClH:1].[CH2:23]([N:26]([N:18]([C:19](=[O:22])[CH3:20])[C:14]1[S:15][C:16]2[C:12](=[CH:11][C:9]3[N:10]=[C:6]([N:5]([N:26]([CH2:27][CH2:28][CH3:29])[CH2:23][CH2:24][CH3:25])[C:3](=[O:4])[CH3:2])[S:7][C:8]=3[CH:17]=2)[N:13]=1)[CH2:27][CH2:28][CH3:29])[CH2:24][CH3:25]

参加物

4

反応物 2

HCID 8902DipropylamineHCID 157546412,6-Bis-(chloroacetyl-amino)benzo[1,2-d:5,4-d']bisthiazole

生成物 1

HCID 705475212,6-Bis-(di-n-propylamino-acetylamino)-benzo[1,2-d:5,4-d']bisthiazole dihydrochloride

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

A mixture of 7.2 gm of 2,6-bis-(chloroacetyl-amino)-benzo[1,2-d:5,4-d']bisthiazole, 10 gm of di-n-propylamine and 100 ml of dioxane was refluxed for two hours and then evaporated to dryness in vacuo. The residue was dissolved in chloroform, and the solution was washed with water, dried, evaporated to a small volume and chromatographed on a 300 gm silicagel column with chloroform and chloroform/methanol (95:5) as the mobile phase. The title compound, 2.5 gm (25.5% of theory), was eluted, dissolved in chloroform, treated with gaseous hydrogen chloride, and the collected hydrochloride was recrystallized from ethanol/water. M.P. 210° C.

後処理

  1. temperaturewas refluxed for two hours
  2. customevaporated to dryness in vacuo
  3. dissolutionThe residue was dissolved in chloroform
  4. washthe solution was washed with water
  5. customdried
  6. customevaporated to a small volume
  7. customchromatographed on a 300 gm silicagel column with chloroform and chloroform/methanol (95:5) as the mobile phase
  8. washThe title compound, 2.5 gm (25.5% of theory), was eluted
  9. dissolutiondissolved in chloroform
  10. additiontreated with gaseous hydrogen chloride
  11. customthe collected hydrochloride was recrystallized from ethanol/water

出典と根拠

ORDレコード
ord-236f0e59dd9e4b9aa9ece27c11f05b3d
出典データセット
uspto-grants-1982_08
特許番号
US04344946

関連ノート

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