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

HRID 66559ノート

反応式

HRID 66559 の反応式
[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

参加物

5

反応物 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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b3907f74c53142b48cdc5f4b528aef75
出典データセット
uspto-grants-1982_08
特許番号
US04342761

反応ノート

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