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Piperidine → HCID 68546659、化合物

HRID 1841881
ノート
印刷プレビュー

反応式

HRID 1841881 の反応式
[C:1]([CH2:3][C:4]([NH:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][C:12]([OH:14])=[O:13])=[O:5])#[N:2].[CH3:15][N:16]([CH3:27])[C:17]1[CH:18]=[C:19]([CH:22]=[CH:23][C:24]=1[O:25][CH3:26])[CH:20]=O.N1CCCCC1>N1C=CC=CC=1>[C:1]([C:3](=[CH:20][C:19]1[CH:22]=[CH:23][C:24]([O:25][CH3:26])=[C:17]([N:16]([CH3:27])[CH3:15])[CH:18]=1)[C:4]([NH:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][C:12]([OH:14])=[O:13])=[O:5])#[N:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8082PiperidineHCID 12225606Benzaldehyde, 3-(dimethylamino)-4-methoxy-HCID 85875172HCID 85875172、化合物

生成物 1

HCID 68546659HCID 68546659、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

3.96 g (20 mMol 6-(2-cyan-acetylamino)hexanoic acid was dissolved in 27 ml pyridine. 3.64 g (20 mMol) 3-dimethylamino-4-methoxybenzaldehyde and 0.6 mL piperidine were added to the solution and the reaction mixture was stirred for 20 hours. After evaporation of the reaction mixture the residue was solved in 150 ml ethyl acetate and 150 ml water and the pH was adjusted with pure acetic acid to 4.2. The aqueous phase was extracted with ethyl acetate. The collected ethyl acetate phases were washed with NaCl-Solution, dried and evaporated. The residue was chromatographed on SiO2 with ethyl acetate under low pressure. The product was crystallized from little ethyl acetate.

後処理

  1. customAfter evaporation of the reaction mixture the residue
  2. extractionThe aqueous phase was extracted with ethyl acetate
  3. washThe collected ethyl acetate phases were washed with NaCl-Solution
  4. customdried
  5. customevaporated
  6. customThe residue was chromatographed on SiO2 with ethyl acetate under low pressure
  7. customThe product was crystallized from little ethyl acetate

出典と根拠

ORDレコード
ord-11b227e362d247d6abe34ac0f6d8f0d4
出典データセット
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08946129B2

反応ノート

読み込み中…

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