ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Piperidine → HCID 66655979、化合物

HRID 1505472
ノート
印刷プレビュー

反応式

HRID 1505472 の反応式
N[C:2]1[C:3]2[C:27]3([CH2:31][CH2:30]OC3)[C:26](=[O:32])[NH:25][C:4]=2[N:5]=[C:6]([C:8]2[C:16]3[C:11](=[N:12][CH:13]=[CH:14][CH:15]=3)[N:10]([CH2:17][C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=3[F:24])[N:9]=2)[N:7]=1.N1CCCC[CH2:34]1>CC(C)=O.C(OCC)(=O)C>[F:24][C:19]1[CH:20]=[CH:21][CH:22]=[CH:23][C:18]=1[CH2:17][N:10]1[C:11]2=[N:12][CH:13]=[CH:14][CH:15]=[C:16]2[C:8]([C:6]2[N:7]=[CH:2][C:3]3[C:27](=[C:31]([CH3:34])[CH3:30])[C:26](=[O:32])[NH:25][C:4]=3[N:5]=2)=[N:9]1
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 2

HCID 8082PiperidineHCID 56598426HCID 56598426、化合物

生成物 1

HCID 66655979HCID 66655979、化合物

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 8857Ethyl Acetate溶媒

実験手順

500 mg (1.388 mmol) of Example 4 were initially charged in acetone (50 ml), 0.274 ml (2.775 mmol) of piperidine was added and the mixture was heated under reflux for 1 h. After cooling, a precipitate was filtered off and washed with acetone, and the filtrate was concentrated under reduced pressure. This residue was then purified by chromatography on silica gel (mobile phase: cyclohexane/ethyl acetate gradient). The material obtained in this manner was once more slurried in ethyl acetate, filtered off, washed with ethyl acetate and dried under high vacuum. This gave 101 mg of the title compound as a solid (18% of theory).

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 1 h
  3. temperatureAfter cooling
  4. filtrationa precipitate was filtered off
  5. washwashed with acetone
  6. concentrationthe filtrate was concentrated under reduced pressure
  7. customThis residue was then purified by chromatography on silica gel (mobile phase: cyclohexane/ethyl acetate gradient)
  8. customThe material obtained in this manner
  9. filtrationfiltered off
  10. washwashed with ethyl acetate
  11. customdried under high vacuum

出典と根拠

ORDレコード
ord-8eebc0489ef9409e9a320a1e9fceff98
出典データセット
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09216978B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート