Triethylamine → 2-([2-(1,4-Benzodioxan-2-yl)-2-hydroxyethyl]piperid-4-yl)-1H-isoindole-1,3-(2H)-dione

HRID 66559노트

반응식

HRID 66559 반응식
[O:1]1[C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=2[O:4][CH2:3][CH:2]1[CH:11]([OH:14])[CH2:12]Br.Cl.[NH:16]1[CH2:21][CH2:20][CH:19]([N:22]2[C:30](=[O:31])[C:29]3[C:24](=[CH:25][CH:26]=[CH:27][CH:28]=3)[C:23]2=[O:32])[CH2:18][CH2:17]1.C(N(CC)CC)C>C(O)C>[O:1]1[C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=2[O:4][CH2:3][CH:2]1[CH:11]([OH:14])[CH2:12][N:16]1[CH2:21][CH2:20][CH:19]([N:22]2[C:23](=[O:32])[C:24]3[C:29](=[CH:28][CH:27]=[CH:26][CH:25]=3)[C:30]2=[O:31])[CH2:18][CH2:17]1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 126085902-Bromo-1-(2,3-dihydro-1,4-benzodioxin-2-yl)ethan-1-olHCID 218825602-(Piperidin-4-yl)isoindoline-1,3-dione hydrochloride

생성물 1

HCID 130189842-([2-(1,4-Benzodioxan-2-yl)-2-hydroxyethyl]piperid-4-yl)-1H-isoindole-1,3-(2H)-dione

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Erythro, 1-(1,4-benzodioxan-2-yl)-2-bromoethanol (1.29 g, 0.005 m) and 2-(piperid-4-yl)-1H-isoindole-1,3-(2H)dione hydrochloride (1.33 g, 0.005 cm3) in ethanol (75 cm3) with triethylamine (3.03 g, 0.03 cm3) were refluxed for 18 hours. The solution was cooled and the solvent evaporated. the residue was dissolved in chloroform and then washed twice with water, dried (MgSO4) and evaporated. The residue was dissolved in isopropyl alcohol and acidified with ethanolic HCl. The crystallised material was filtered to give the title compound as the hydrochloride salt m.p. 235°-237° C.

후처리

  1. temperatureThe solution was cooled
  2. customthe solvent evaporated
  3. dissolutionthe residue was dissolved in chloroform
  4. washwashed twice with water
  5. dry with materialdried (MgSO4)
  6. customevaporated
  7. dissolutionThe residue was dissolved in isopropyl alcohol
  8. filtrationThe crystallised material was filtered

출처 및 근거

ORD 기록
ord-b3907f74c53142b48cdc5f4b528aef75
출처 데이터셋
uspto-grants-1982_08
특허 번호
US04342761

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