Dimethylformamide → HCID 19917189、化合物

HRID 1756199ノート

反応式

HRID 1756199 の反応式
[OH:1][C:2]1[C:14]([CH2:15][CH:16]=[CH2:17])=[C:13]([OH:18])[CH:12]=[CH:11][C:3]=1[C:4]([N:6]1[CH2:10][CH2:9][CH2:8][CH2:7]1)=[O:5].I[CH2:20][CH2:21][CH2:22][O:23][C:24]1[CH:37]=[CH:36][C:27]2[CH2:28][CH2:29][CH:30]([C:32]([O:34][CH3:35])=[O:33])[O:31][C:26]=2[C:25]=1CCC.C(=O)([O-])[O-].[K+].[K+].[CH3:47]N(C=O)C.C(O[CH2:56][CH3:57])(=O)C>>[CH3:35][O:34][C:32]([C:30]1([CH2:47][CH2:56][CH3:57])[CH2:29][CH2:28][C:27]2[CH:36]=[CH:37][C:24]([O:23][CH2:22][CH2:21][CH2:20][O:18][C:13]3[CH:12]=[CH:11][C:3]([C:4]([N:6]4[CH2:10][CH2:9][CH2:8][CH2:7]4)=[O:5])=[C:2]([OH:1])[C:14]=3[CH2:15][CH:16]=[CH2:17])=[CH:25][C:26]=2[O:31]1)=[O:33]

参加物

6

反応物 5

HCID 6228DimethylformamideHCID 8857Ethyl AcetateHCID 11430Potassium CarbonateHCID 14722828HCID 14722828、化合物HCID 15341804HCID 15341804、化合物

生成物 1

HCID 19917189HCID 19917189、化合物

実験手順

1-[2,4-Dihydroxy-3-(2-propenyl)benzoyl]pyrrolidine (260 mg, 1.05 mmol), the compound of Example 23 (440 mg, 1.05 mmol), and potassium carbonate (350 mg, 2.4 mmol) were added to about 15 to 20 ml of DMF, and the reaction mixture was stirred at room temperature overnight. The reaction mixture was diluted with ethyl acetate and washed with water. The organic layer was dried over magnesium sulfate and concentrated under vacuum. Chromatography of the crude material on silica gel using 20% ethyl acetate/hexane as eluant gave the product.

後処理

  1. washwashed with water
  2. dry with materialThe organic layer was dried over magnesium sulfate
  3. concentrationconcentrated under vacuum

出典と根拠

ORDレコード
ord-fb9b25e377ad4e59aa21e5913493ca4e
出典データセット
uspto-grants-1995_08
特許番号
US05439937

反応ノート

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