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

HRID 911085ノート

反応式

HRID 911085 の反応式
[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]

参加物

4

反応物 2

HCID 24408BromineHCID 27772501,4-Diacetylpiperidine

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-af048f9ba91947b9ae486612e35e08d6
出典データセット
uspto-grants-2011_09
特許番号
US08022222B2

反応ノート

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