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

Sodium Bicarbonate → 1-(2,4-dichlorophenyl)-4-(4-oxopiperidin-1-yl)-2,3,6-trimethyl-1H-pyrrolo[2,3-b]pyridine

HRID 23546
ノート
印刷プレビュー

反応式

HRID 23546 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[N:9]1[C:13]2=[N:14][C:15]([CH3:28])=[CH:16][C:17]([N:18]3[CH2:27][CH2:26][C:21]4(OCC[O:22]4)[CH2:20][CH2:19]3)=[C:12]2[C:11]([CH3:29])=[C:10]1[CH3:30].C(=O)([O-])O.[Na+]>Cl.O1CCCC1>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[N:9]1[C:13]2=[N:14][C:15]([CH3:28])=[CH:16][C:17]([N:18]3[CH2:27][CH2:26][C:21](=[O:22])[CH2:20][CH2:19]3)=[C:12]2[C:11]([CH3:29])=[C:10]1[CH3:30]
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 516892Sodium BicarbonateHCID 12134654HCID 12134654、化合物

生成物 1

HCID 121346551-(2,4-dichlorophenyl)-4-(4-oxopiperidin-1-yl)-2,3,6-trimethyl-1H-pyrrolo[2,3-b]pyridine収率 81.6%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒2 回HCID 8028Tetrahydrofuran溶媒

実験手順

After 1-(2,4-dichlorophenyl)-4-(1,4-dioxa-8-azaspiro[4.5]dec-8-yl)-2,3,6-trimethyl-1H-pyrrolo[2,3-b]-pyridine (5.21 g) was stirred in a mixture of 4 M hydrochloric acid (60 mL) and tetrahydrofuran (60 mL) at room temperature for 2.5 hours, 6 M hydrochloric acid (30 mL) was added thereto and the resulting mixture was stirred overnight. After completion of the reaction, the reaction mixture was poured into a saturated aqueous sodium hydrogen-carbonate solution and extracted three times with ethyl acetate. The combined organic layer was dried over anhydrous sodium sulfate, after which the desiccating agent was filtered off and the filtrate was concentrated under reduced pressure. The crystals thus obtained were washed with ethyl acetate to obtain 1-(2,4-dichlorophenyl)-4-(4-oxopiperidin-1-yl)-2,3,6-trimethyl-1H-pyrrolo[2,3-b]pyridine (3.83 g).

後処理

  1. customAfter completion of the reaction
  2. extractionextracted three times with ethyl acetate
  3. dry with materialThe combined organic layer was dried over anhydrous sodium sulfate
  4. filtrationafter which the desiccating agent was filtered off
  5. concentrationthe filtrate was concentrated under reduced pressure
  6. customThe crystals thus obtained
  7. washwere washed with ethyl acetate

出典と根拠

ORDレコード
ord-caac4ca01fad401d8a0672d766d57787
出典データセット
uspto-grants-2005_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06852732B2

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