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

Potassium Carbonate → Tert-butyl {2-[4-(5-chloro-3-phenyl-1,6-naphthyridin-2-yl)phenyl]-5,8-dioxaspiro[3.4]oct-2-yl]carbamate

HRID 221976
ノート
印刷プレビュー

反応式

HRID 221976 の反応式
C1(CC([C:10]2[CH:15]=[CH:14][C:13]([C:16]3([NH:24][C:25](=[O:31])[O:26][C:27]([CH3:30])([CH3:29])[CH3:28])[CH2:19][C:18]4([O:23][CH2:22][CH2:21][O:20]4)[CH2:17]3)=[CH:12][CH:11]=2)=O)C=CC=CC=1.C(=O)([O-])[O-].[K+].[K+].[Cl:38][C:39]1[C:44]([CH:45]=O)=[C:43]([NH:47][C:48](=O)OC(C)(C)C)[CH:42]=[CH:41][N:40]=1.C(=O)(O)[O-].[Na+]>CN(C=O)C>[Cl:38][C:39]1[N:40]=[CH:41][CH:42]=[C:43]2[C:44]=1[CH:45]=[C:16]([C:13]1[CH:14]=[CH:15][CH:10]=[CH:11][CH:12]=1)[C:48]([C:10]1[CH:15]=[CH:14][C:13]([C:16]3([NH:24][C:25](=[O:31])[O:26][C:27]([CH3:30])([CH3:29])[CH3:28])[CH2:19][C:18]4([O:20][CH2:21][CH2:22][O:23]4)[CH2:17]3)=[CH:12][CH:11]=1)=[N:47]2
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 11430Potassium CarbonateHCID 516892Sodium BicarbonateHCID 52987944tert-Butyl (2-chloro-3-formylpyridin-4-yl)carbamateHCID 59161539HCID 59161539、化合物

生成物 1

HCID 59161532Tert-butyl {2-[4-(5-chloro-3-phenyl-1,6-naphthyridin-2-yl)phenyl]-5,8-dioxaspiro[3.4]oct-2-yl]carbamate

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

反応条件

温度
80 °C

実験手順

To a solution of tert-butyl {2-[4-(phenylacetyl)phenyl]-5,8-dioxaspiro[3.4]oct-2-yl}carbamate (1-7) (8.8 g, 20.8 mmol) in DMF (100 mL) was added potassium carbonate (14.4 g, 104 mmol) and tert-butyl (2-chloro-3-formyl-4-pyridinyl)carbamate (1-8) (5.33 g, 20.8 mmol) and the reaction mixture was heated 80° C. over night. The reaction mixture was poured into saturated sodium bicarbonate, extracted with EtOAc, dried over sodium sulfate, filtered and concentrated. The crude residue was purified by column chromatography eluting with 1-80% EtOAc/Hexane. The appropriate fractions were combined and the solvent removed in vacuo to give tert-butyl {2-[4-(5-chloro-3-phenyl-1,6-naphthyridin-2-yl)phenyl]-5,8-dioxaspiro[3.4]oct-2-yl}carbamate (1-9). MS (M+H)+: 545.

後処理

  1. extractionextracted with EtOAc
  2. dry with materialdried over sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customThe crude residue was purified by column chromatography
  6. washeluting with 1-80% EtOAc/Hexane
  7. customthe solvent removed in vacuo

出典と根拠

ORDレコード
ord-d6e671ed5feb4a2fa45bd4642b1c2797
出典データセット
uspto-grants-2012_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08207169B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート