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1-(2,2-dimethylpropanoyl)piperazine → HCID 66907079、化合物

HRID 1690634
ノート
印刷プレビュー

反応式

HRID 1690634 の反応式
[CH3:1][C:2]([CH3:12])([CH3:11])[C:3]([N:5]1[CH2:10][CH2:9][NH:8][CH2:7][CH2:6]1)=[O:4].[CH2:13]([O:15][C:16](=[O:38])[CH2:17][CH2:18][C:19]1[CH:24]=[CH:23][C:22]([C:25]2[CH:30]=[CH:29][C:28]([CH:31]=O)=[CH:27][CH:26]=2)=[C:21]([O:33]CCOC)[CH:20]=1)[CH3:14]>C1COCC1>[CH2:13]([O:15][C:16](=[O:38])[CH2:17][CH2:18][C:19]1[CH:24]=[CH:23][C:22]([C:25]2[CH:30]=[CH:29][C:28]([CH2:31][N:8]3[CH2:9][CH2:10][N:5]([C:3](=[O:4])[C:2]([CH3:12])([CH3:11])[CH3:1])[CH2:6][CH2:7]3)=[CH:27][CH:26]=2)=[C:21]([O:33][CH2:18][CH2:17][CH2:16][O:15][CH3:13])[CH:20]=1)[CH3:14]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 27614081-(2,2-dimethylpropanoyl)piperazineHCID 86761547HCID 86761547、化合物

生成物 1

HCID 66907079HCID 66907079、化合物収率 153.6%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a solution of 2,2-dimethyl-1-piperazin-1-yl-propan-1-one (37.45 mg, 0.22 mmol) in THF (2 mL) concentrated acetic acid (63 μL, 1.1 mmol), Ethyl-3-[4′-Formyl-2-(2-methoxy-ethoxy)-biphenyl-4-yl]-propionate (74 mg, 0.2 mmol) dissolved in THF (1 mL) and cyanoborhydride resin (123 mg, 0.3 mmol) was added. The reaction was shaken in a closed-vessel under argon at r.t. overnight. The mixture was filtered and dried under reduced pressure. The residue was redissolved in ethyl acetate (20 mL) and washed with an aqueous sodium hydrogen carbonate solution (20 mL). The organic layer was separated, dried over sodium sulfate, filtered and dried under reduced pressure to give 80.6 mg of the titled compound.

後処理

  1. filtrationThe mixture was filtered
  2. customdried under reduced pressure
  3. dissolutionThe residue was redissolved in ethyl acetate (20 mL)
  4. washwashed with an aqueous sodium hydrogen carbonate solution (20 mL)
  5. customThe organic layer was separated
  6. dry with materialdried over sodium sulfate
  7. filtrationfiltered
  8. customdried under reduced pressure

出典と根拠

ORDレコード
ord-199d1d5dc1414ac6826f53e3168276c6
出典データセット
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08153647B2

反応ノート

読み込み中…

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