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

Dichloromethane → HCID 22100931、化合物

HRID 1458365
ノート
印刷プレビュー

反応式

HRID 1458365 の反応式
[CH3:1][C:2]1[CH:3]=[C:4]([C:9]2[NH:10][C:11]3[C:16]([CH:17]=2)=[CH:15][CH:14]=[CH:13][CH:12]=3)[CH:5]=[C:6]([CH3:8])[CH:7]=1.[C:18](Cl)(=[O:22])[C:19](Cl)=[O:20].Cl.Cl.[NH:26]1[CH2:31][CH2:30][CH:29]([C:32]2[CH:37]=[CH:36][N:35]=[CH:34][CH:33]=2)[CH2:28][CH2:27]1.C(Cl)Cl>C(OCC)(=O)C.C(N(CC)CC)C>[CH3:1][C:2]1[CH:3]=[C:4]([C:9]2[NH:10][C:11]3[C:16]([C:17]=2[C:18](=[O:22])[C:19]([N:35]2[CH2:36][CH2:37][CH:32]([C:29]4[CH:28]=[CH:27][N:26]=[CH:31][CH:30]=4)[CH2:33][CH2:34]2)=[O:20])=[CH:15][CH:14]=[CH:13][CH:12]=3)[CH:5]=[C:6]([CH3:8])[CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 6344DichloromethaneHCID 65578Oxalyl chlorideHCID 221008754-(Piperidin-4-yl)pyridine dihydrochlorideHCID 22100925HCID 22100925、化合物

生成物 1

HCID 22100931HCID 22100931、化合物

試薬・触媒・溶媒 2

HCID 8471Triethylamine溶媒
HCID 8857
Ethyl Acetate
溶媒

実験手順

To a solution of 2-(3,5-dimethylphenyl)-1H-indole (200 mg in 2 mL dry methylene chloride) was added dropwise 0.083 mL oxalyl chloride and the mixture stirred at room temperature. After 1 hour, 213 mg 1,2,3,4,5,6-hexahydro-[4,4']bipyridinyl dihydrochloride was added followed by 1.5 mL methylene chloride and 0.567 mL triethylamine and the mixture continued stirring at room temperature. After 4 hours the reaction was diluted with ethyl acetate and washed sequentially with water, saturated aqueous ammonium chloride and brine. The organic portion was dried over sodium sulfate and the concentrate purified by flash chromatography on silica gel (methylene chloride:methanol, 96:4) to give the title compound (148 mg).

後処理

  1. stirringthe mixture continued stirring at room temperature
  2. washwashed sequentially with water, saturated aqueous ammonium chloride and brine
  3. dry with materialThe organic portion was dried over sodium sulfate
  4. customthe concentrate purified by flash chromatography on silica gel (methylene chloride:methanol, 96:4)

出典と根拠

ORDレコード
ord-486bc19facc24dbba06c60338d74599b
出典データセット
uspto-grants-1998_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05849764

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