Hydrochloric Acid → HCID 13363395, 화합물

HRID 484717노트

반응식

HRID 484717 반응식
[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Cl-].[Al+3].[Cl-].[Cl-].[C:12]([N:15]1[CH2:20][CH2:19][CH:18]([C:21](Cl)=[O:22])[CH2:17][CH2:16]1)(=[O:14])[CH3:13].Cl>>[C:12]([N:15]1[CH2:16][CH2:17][CH:18]([C:21](=[O:22])[C:5]2[CH:6]=[CH:7][C:2]([Br:1])=[CH:3][CH:4]=2)[CH2:19][CH2:20]1)(=[O:14])[CH3:13]

참가 물질

5

반응물 4

HCID 313Hydrochloric AcidHCID 7961BromobenzeneHCID 1009501-Acetylpiperidine-4-carbonyl chlorideHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 13363395HCID 13363395, 화합물수율 34%

실험 절차

To a stirred and warm (40° C.) mixture of 600 parts of bromobenzene and 223 parts of aluminum chloride were added portionwise 168.8 parts of 1-acetyl-4-piperidinecarbonyl chloride. Upon completion, stirring was continued for 1 hour at 50° C. and overnight at room temperature. The reaction mixture was poured onto a mixture of 1500 parts of crushed ice and hydrogen chloride. The whole was stirred thoroughly. The precipitated product was filtered off, washed with 2,2'-oxybispropane and dissolved in a mixture of 2250 parts of trichloromethane and 200 parts of water. The layers were separated. The organic layer was dried, filtered and evaporated. The solid residue was suspended in 280 parts of 2,2'-oxybispropane. The product was filtered off and dried, yielding 94 parts (34%) of 1-acetyl-4-(4-bromobenzoyl)piperidine; mp. 120° C. (intermediate 15).

후처리

  1. temperaturewarm
  2. stirringUpon completion, stirring
  3. stirringThe whole was stirred thoroughly
  4. filtrationThe precipitated product was filtered off
  5. washwashed with 2,2'-oxybispropane
  6. dissolutiondissolved in a mixture of 2250 parts of trichloromethane and 200 parts of water
  7. customThe layers were separated
  8. customThe organic layer was dried
  9. filtrationfiltered
  10. customevaporated
  11. filtrationThe product was filtered off
  12. customdried

출처 및 근거

ORD 기록
ord-b3264ca2cf2244909dae3851da097535
출처 데이터셋
uspto-grants-1985_08
특허 번호
US04533665

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