Hydrochloric Acid → (4-Fluorophenyl)(piperazin-1-yl)methanone

HRID 1381110노트

반응식

HRID 1381110 반응식
Cl.[NH:2]1[CH2:7][CH2:6][NH:5][CH2:4][CH2:3]1.[F:8][C:9]1[CH:17]=[CH:16][C:12]([C:13](Cl)=[O:14])=[CH:11][CH:10]=1.C([O-])(=O)C.[Na+].C(=O)([O-])[O-].[K+].[K+]>O>[F:8][C:9]1[CH:17]=[CH:16][C:12]([C:13]([N:2]2[CH2:7][CH2:6][NH:5][CH2:4][CH2:3]2)=[O:14])=[CH:11][CH:10]=1

참가 물질

7

반응물 5

HCID 313Hydrochloric AcidHCID 4837PiperazineHCID 11430Potassium CarbonateHCID 678794-Fluorobenzoyl chlorideHCID 517045Sodium Acetate

생성물 1

HCID 771862(4-Fluorophenyl)(piperazin-1-yl)methanone수율 88%

시약·촉매·용매 1

HCID 962Water용매2회

반응 조건

온도
50 °C

실험 절차

Concentrated hydrochloric acid was added dropwise to a solution of piperazine (0.124 mol) in water (110 ml) to adjust the pH to 2.8. The solution was then heated to 50° C. 4-Fluorobenzoyl chloride (0.124 mol) was added to the warm solution dropwise while maintaining the pH at 2.8 by the concurrent addition of 40% aqueous sodium acetate solution. After complete addition, a solution of potassium carbonate (47 g) in water (50 ml) was added and the mixture cooled in an ice bath. The cold mixture was extracted with chloroform (5×150 ml). The combined extracts were dried (MgSO4) and evaporated in vacuo affording 22.5 g of a white solid (88% yield). Spectral data are consistent with the assigned structure. This material was used without further purification.

후처리

  1. temperaturewhile maintaining the pH at 2.8
  2. additionAfter complete addition
  3. temperaturethe mixture cooled in an ice bath
  4. extractionThe cold mixture was extracted with chloroform (5×150 ml)
  5. dry with materialThe combined extracts were dried (MgSO4)
  6. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-9be599ad3d2b4140bc2451d2d3e8332c
출처 데이터셋
uspto-grants-1986_04
특허 번호
US04585773

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