Dimethylformamide → HCID 19917189、化合物

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

反応物 5

HCID 6228Dimethylformamide

HCID 8857Ethyl Acetate

HCID 11430Potassium Carbonate

HCID 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

washwashed with water
dry with materialThe organic layer was dried over magnesium sulfate
concentrationconcentrated under vacuum

出典と根拠

ORDレコード: ord-8dd72f8c877e43ad918a613b20716e6d
出典データセット: uspto-grants-1994_05
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US05310951

反応ノート

読み込み中…