Potassium Carbonate → HCID 13330057、化合物

HRID 846178ノート

反応式

HRID 846178 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:19]=[CH:20][C:21]=1[O:22][CH3:23])[C:6]([C@H:8]1[CH2:12][CH2:11][CH2:10][N:9]1[C:13](=[O:18])[C:14]([F:17])([F:16])[F:15])=O.C([SiH](CC)CC)C.C(=O)([O-])[O-].[K+].[K+]>C(Cl)Cl>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:19]=[CH:20][C:21]=1[O:22][CH3:23])[CH2:6][C@H:8]1[CH2:12][CH2:11][CH2:10][N:9]1[C:13](=[O:18])[C:14]([F:17])([F:15])[F:16]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 12052TriethylsilaneHCID 13330049HCID 13330049、化合物

生成物 1

HCID 13330057HCID 13330057、化合物収率 68%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

(R)-2-(3,4-dimethoxybenzoyl)-1-trifluoroacetylpyrrolidine (4.9 g, 0.015 mol) was dissolved in 50 mL dry CH2Cl2 in a 500 mL round-bottom flask. To the solution was added triethylsilane (20 g, 0.172 mol) and BF3 ·Et2O (50 mL). The reaction mixture was stirred at room temperature for 3 days, after which time a saturated aqueous solution of potassium carbonate was added cautiously in a dropwise manner. When no more gas was evolved, 100 mL CH2Cl2 was added. The mixture was then shaken. The triphasic mixture was filtered through a glass fritted funnel, and the organic layer separated and dried with MgSO4. Removal of the solvent in vacuo yielded 3.2 g of (R)-2-(3,4-dimethoxybenzyl)-1-trifluoroacetylpyrrolidine (68% yield), as an oil which could be used without further purification.

後処理

  1. stirringThe mixture was then shaken
  2. filtrationThe triphasic mixture was filtered through a glass fritted funnel
  3. customthe organic layer separated
  4. dry with materialdried with MgSO4
  5. customRemoval of the solvent in vacuo

出典と根拠

ORDレコード
ord-652b965da8da401594f56b8fdc478665
出典データセット
uspto-grants-1992_08
特許番号
US05135944

反応ノート

読み込み中…