1,1'-Carbonyldiimidazole → 1-(1,4-Benzodioxan-2-yl-acetyl)-4-ethoxy-4-phenylpiperidine

HRID 1391068ノート

反応式

HRID 1391068 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[CH2:11][C:12]([OH:14])=O.C(N1C=CN=C1)(N1C=CN=C1)=O.[CH2:27]([O:29][C:30]1([C:36]2[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=2)[CH2:35][CH2:34][NH:33][CH2:32][CH2:31]1)[CH3:28]>O1CCCC1>[O:1]1[C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=2[O:4][CH2:3][CH:2]1[CH2:11][C:12]([N:33]1[CH2:34][CH2:35][C:30]([O:29][CH2:27][CH3:28])([C:36]2[CH:37]=[CH:38][CH:39]=[CH:40][CH:41]=2)[CH2:31][CH2:32]1)=[O:14]

参加物

5

反応物 3

HCID 682631,1'-CarbonyldiimidazoleHCID 2675342,3-Dihydro-1,4-benzodioxin-2-acetic acidHCID 4173924-Ethoxy-4-phenylpiperidinium chloride

生成物 1

HCID 213319941-(1,4-Benzodioxan-2-yl-acetyl)-4-ethoxy-4-phenylpiperidine

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

The starting material is prepared as follows: To the solution of 3.3 g of 1,4-benzodioxan-2-yl-acetic acid in 30 ml of tetrahydrofuran, 3.1 g of 1,1'-carbonyldiimidazole are added while stirring followed, after 30 minutes, by 3.5 g of 4-ethoxy-4-phenylpiperidine in 30 ml of tetrahydrofuran. The mixture is stirred for 18 hours at room temperature, evaporated and the residue taken up in ethyl acetate. The solution is washed with water, N hydrochloric acid and saturated aqueous sodium chloride, dried and evaporated, to yield the 1-(1,4-benzodioxan-2-yl-acetyl)-4-ethoxy-4-phenylpiperidine.

後処理

  1. customThe starting material is prepared
  2. stirringThe mixture is stirred for 18 hours at room temperature
  3. customevaporated
  4. washThe solution is washed with water, N hydrochloric acid and saturated aqueous sodium chloride
  5. customdried
  6. customevaporated

出典と根拠

ORDレコード
ord-5b9cef8180d24d8985419b3103e05fe7
出典データセット
uspto-grants-1979_02
特許番号
US04140781

反応ノート

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