Sodium Carbonate → HCID 22325082, 화합물

HRID 496068노트

반응식

HRID 496068 반응식
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

참가 물질

6

반응물 4

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

생성물 1

HCID 22325082HCID 22325082, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-4f633adeb4f54805b77d3efdb5a8a4ef
출처 데이터셋
uspto-grants-2005_09
특허 번호
US06943184B2

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