Sodium Carbonate → HCID 22325082、化合物

HRID 496068ノート

反応式

HRID 496068 の反応式
F[B-](F)(F)F.[CH2:6]([O+](CC)CC)[CH3:7].[N:13]1([C:18]2([C:21](N)=[O:22])[CH2:20][CH2:19]2)[CH2:17][CH2:16][CH2:15][CH2:14]1.P([O-])([O-])(O)=[O:25].[Na+].[Na+].C(=O)([O-])[O-].[Na+].[Na+]>ClCCl>[N:13]1([C:18]2([C:21]([O:22][CH2:6][CH3:7])=[O:25])[CH2:20][CH2:19]2)[CH2:17][CH2:16][CH2:15][CH2:14]1

参加物

6

反応物 4

HCID 10340Sodium CarbonateHCID 24203Sodium Phosphate, DibasicHCID 2723982Triethyloxonium tetrafluoroborateHCID 223251301-(Pyrrolidin-1-yl)cyclopropanecarboxamide

生成物 1

HCID 22325082HCID 22325082、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A solution containing 11.4 g of triethyloxonium tetrafluoroborate and 40 ml of dichloromethane is added dropwise, at 0° C., to a suspension containing 1.54 g of the product obtained in Step 2, 10 g of disodium hydrogen phosphate and 120 ml of dichloromethane. After 20 hours at 20° C., 40 ml of 10% aqueous sodium carbonate solution are added. The mixture is separated and the aqueous phase is extracted with dichloromethane. The combined organic phases are dried over sodium sulphate and then concentrated to dryness. The residue is taken up in 1N aqueous hydrochloric acid and the resulting solution is left at 20° C. for 3 hours. The mixture is made alkaline with sodium carbonate and extracted with dichloromethane. The combined dichloromethane phases are dried over sodium sulphate and concentrated to dryness. Chromatography over silica gel (dichloromethane/tetrahydrofuran: 95/5) allows the desired product to be isolated.

後処理

  1. additionis added dropwise, at 0° C., to a suspension
  2. customThe mixture is separated
  3. extractionthe aqueous phase is extracted with dichloromethane
  4. dry with materialThe combined organic phases are dried over sodium sulphate
  5. concentrationconcentrated to dryness
  6. waitthe resulting solution is left at 20° C. for 3 hours
  7. extractionextracted with dichloromethane
  8. dry with materialThe combined dichloromethane phases are dried over sodium sulphate
  9. concentrationconcentrated to dryness
  10. customto be isolated

出典と根拠

ORDレコード
ord-4f633adeb4f54805b77d3efdb5a8a4ef
出典データセット
uspto-grants-2005_09
特許番号
US06943184B2

反応ノート

読み込み中…