Piperidine → HCID 89869680、化合物

HRID 1755482ノート

反応式

HRID 1755482 の反応式
C1C2C(COC(=O)[NH:17][C@@H:18]([CH3:42])[C:19](=[O:41])[NH:20][C@@H:21]([CH2:33][C:34]3[CH:39]=[CH:38][C:37]([OH:40])=[CH:36][CH:35]=3)[C:22](=[O:32])[NH:23][CH2:24][C:25]([O:27][C:28]([CH3:31])([CH3:30])[CH3:29])=[O:26])C3C(=CC=CC=3)C=2C=CC=1.N1CCCCC1>CN(C=O)C>[NH2:17][C@@H:18]([CH3:42])[C:19]([NH:20][C@@H:21]([CH2:33][C:34]1[CH:39]=[CH:38][C:37]([OH:40])=[CH:36][CH:35]=1)[C:22]([NH:23][CH2:24][C:25]([O:27][C:28]([CH3:29])([CH3:30])[CH3:31])=[O:26])=[O:32])=[O:41]

参加物

4

反応物 2

HCID 8082PiperidineHCID 89869677HCID 89869677、化合物

生成物 1

HCID 89869680HCID 89869680、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a solution of material from Example 99 (577 mg, 0.579 mmol) in anhydrous DMF (4 mL) is added piperidine (1 mL, 10.1 mmol). The resulting solution is stirred at room temp for 20 min, then the solvent is removed in vacuo. The resulting solid is evaporated sequentially from ethyl acetate, 1,2-dichloroethane and dichloromethane and dried under high vacuum for several hours to give the title compound as a white solid in quantitative yield that contains 1 equivalent of 1-((9H-fluoren-9-yl)methyl)piperidine as a side product. LC/MS (Condition A): ret. T=4.05 min, (M+H)+ 366.

後処理

  1. customthe solvent is removed in vacuo
  2. customThe resulting solid is evaporated sequentially from ethyl acetate, 1,2-dichloroethane and dichloromethane
  3. customdried under high vacuum for several hours

出典と根拠

ORDレコード
ord-935231ace1cd4fc98bb0488045dfb424
出典データセット
uspto-grants-2015_10
特許番号
US09169295B2

反応ノート

読み込み中…