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

HRID 67107

반응식

HRID 67107 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-236f0e59dd9e4b9aa9ece27c11f05b3d
출처 데이터셋
uspto-grants-1982_08
특허 번호
US04344946

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