Hydrochloric Acid → 1-(2-Furoyl)piperazine

HRID 343272노트

반응식

HRID 343272 반응식
O.O.O.O.O.O.[NH:7]1[CH2:12][CH2:11][NH:10][CH2:9][CH2:8]1.Cl.[O:14]1[CH:18]=[CH:17][CH:16]=[C:15]1[C:19](Cl)=[O:20].[OH-].[Na+]>O>[O:14]1[CH:18]=[CH:17][CH:16]=[C:15]1[C:19]([N:7]1[CH2:12][CH2:11][NH:10][CH2:9][CH2:8]1)=[O:20]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 14798Sodium Hydroxide2회HCID 682422-Furancarbonyl chlorideHCID 120181Piperazine, hexahydrate

생성물 1

HCID 5502061-(2-Furoyl)piperazine수율 60%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

This compound and its preparation has been described in Great Britain Patents 1,390,014 and 1,390,015. Piperazine hexahydrate (194 g, 1 mole) was dissolved in 250 ml H2O. The solution was acidified to pH 4.5 with 6N HCl. Furoyl chloride (130.5 g, 1 mole, Aldrich) was added along with 10% NaOH solution at such a rate that the pH was maintained at 4.5. After 1 hour, the solution was made basic (pH=8.5) with NaOH solution. The reaction mixture was continuously extracted with chloroform for 36 hours. The CHCl3 extract was dried over MgSO4, and filtered. Distillation gave 108.2 g product (60%), b.p. 132°-138° C./0.6 mm Hg, m.p. 69°-70° C.

후처리

  1. customThis compound and its preparation
  2. temperaturewas maintained at 4.5
  3. extractionThe reaction mixture was continuously extracted with chloroform for 36 hours
  4. extractionThe CHCl3 extract
  5. dry with materialwas dried over MgSO4
  6. filtrationfiltered
  7. distillationDistillation

출처 및 근거

ORD 기록
ord-82c6f48e8cf44601ac4c07201fdf6858
출처 데이터셋
uspto-grants-1999_01
특허 번호
US05861309

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