Bromine → HCID 18180157, 화합물

HRID 1358937

반응식

HRID 1358937 반응식
[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([C:8]2[CH:13]=[CH:12][CH:11]=[C:10]([N+:14]([O-:16])=[O:15])[CH:9]=2)[CH2:4][CH2:3]1.[Br:17]Br>C(O)(=O)C>[Br:17][C:11]1[CH:12]=[CH:13][C:8]([N:5]2[CH2:6][CH2:7][N:2]([CH3:1])[CH2:3][CH2:4]2)=[CH:9][C:10]=1[N+:14]([O-:16])=[O:15]

참가 물질

4

반응물 2

HCID 24408BromineHCID 121521611-Methyl-4-(3-nitrophenyl)piperazine

생성물 1

HCID 18180157HCID 18180157, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

A solution of 1-methyl-4-(3-nitrophenyl)piperazine (EP0533267A) (1.0 g; 4.5 mmol) in glacial acetic acid (25 ml) was treated with bromine (0.23 ml; 1 equivalent). The reaction mixture was stirred at 75° overnight, then cooled, filtered, and the yellow sticky solid was partitioned between potassium carbonate (aq) and 2% methanol in dichloromethane. The organic phase was dried (Na2SO4) and evaporated under reduced pressure to leave the title compound (D26) as a viscous orange oil (928 mg, 68%) MH+=300/302.

후처리

  1. temperaturecooled
  2. filtrationfiltered
  3. customthe yellow sticky solid was partitioned between potassium carbonate (aq) and 2% methanol in dichloromethane
  4. dry with materialThe organic phase was dried (Na2SO4)
  5. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-04855d2480d14a2993f4accedabd3821
출처 데이터셋
uspto-grants-2003_07
특허 번호
US06599904B2

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