Bromine → 1-(1-Acetylpiperidin-4-yl)-2-bromoethan-1-one

HRID 911085노트

반응식

HRID 911085 반응식
[N:1]1([C:10](=[O:12])[CH3:11])[CH2:6][CH2:5][CH:4]([C:7](=[O:9])[CH3:8])[CH2:3][CH2:2]1.[Br:13]Br>CO>[C:10]([N:1]1[CH2:6][CH2:5][CH:4]([C:7](=[O:9])[CH2:8][Br:13])[CH2:3][CH2:2]1)(=[O:12])[CH3:11]

참가 물질

4

반응물 2

HCID 24408BromineHCID 27772501,4-Diacetylpiperidine

생성물 1

HCID 772303261-(1-Acetylpiperidin-4-yl)-2-bromoethan-1-one수율 80.23%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

1,1′-(Piperidine-1,4-diyl)diethanone (38.00 g, 224.6 mmol) was dissolved in methanol (700 ml) and bromine (12.11 ml, 235.8 mmol) was added in portions. The resulting mixture was agitated 3 hours and the solvent was removed in vacuo. The resulting solid was triturated with ethyl acetate and partitioned between ethyl acetate and sodium carbonate solution. The organic phase was separated, washed with brine, dried and evaporated to give the desired product (44.70 g, 80.23% yield) as yellow solid.

후처리

  1. customthe solvent was removed in vacuo
  2. customThe resulting solid was triturated with ethyl acetate
  3. custompartitioned between ethyl acetate and sodium carbonate solution
  4. customThe organic phase was separated
  5. washwashed with brine
  6. customdried
  7. customevaporated

출처 및 근거

ORD 기록
ord-af048f9ba91947b9ae486612e35e08d6
출처 데이터셋
uspto-grants-2011_09
특허 번호
US08022222B2

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