4-(Piperidin-1-ylmethyl)aniline → HCID 178487200、化合物

HRID 2236612ノート

反応式

HRID 2236612 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[C:9](=[O:13])[NH:8][C:7](=[O:14])/[C:6]/2=[CH:15]/OC.[N:18]1([CH2:24][C:25]2[CH:30]=[CH:29][C:28]([NH2:31])=[CH:27][CH:26]=2)[CH2:23][CH2:22][CH2:21][CH2:20][CH2:19]1>CN(C)C=O>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[C:9](=[O:13])[NH:8][C:7](=[O:14])[C:6]2=[CH:15][NH:31][C:28]1[CH:27]=[CH:26][C:25]([CH2:24][N:18]2[CH2:23][CH2:22][CH2:21][CH2:20][CH2:19]2)=[CH:30][CH:29]=1

参加物

4

反応物 2

HCID 8461504-(Piperidin-1-ylmethyl)anilineHCID 59299827(4E)-6-methoxy-4-methoxymethylene-4H-isoquinoline-1,3-dione

生成物 1

HCID 178487200HCID 178487200、化合物収率 78%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
110 °C

実験手順

A mixture of (4E)-6-methoxy-4-methoxymethylene-4H-isoquinoline-1,3-dione (117 mg, 0.50 mmole), N,N-dimethylformamide (1 mL) and 4-piperidin-1-ylmethyl-phenylamine (95 mg, 0.50 mmole) is stirred and heated at 110° C. for one hour, cooled in the refrigerator overnight. The reaction mixture is evaporated to dryness, taken up in 7.5% methanol in chloroform and passed through a short pad of Florisil eluting with 7.5% methanol in chloroform. The eluate is evaporated in vacuo, treated with acetonitrile, filtered and dried to give a yellow solid 152 mg (78%), mp 272-5° C. dec; MS (ESI): m/z 392.4 (M+H).

後処理

  1. temperaturecooled in the refrigerator overnight
  2. customThe reaction mixture is evaporated to dryness
  3. customThe eluate is evaporated in vacuo
  4. additiontreated with acetonitrile
  5. filtrationfiltered
  6. customdried

出典と根拠

ORDレコード
ord-c51f6884faf54bb88ab5262fe55f2197
出典データセット
uspto-grants-2010_05
特許番号
US07713994B2

反応ノート

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