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

1,3-Propanediol → HCID 11153793、化合物

HRID 644506
ノート
印刷プレビュー

反応式

HRID 644506 の反応式
[CH2:1]([O:3][C:4]([C:6]1[CH:20]=[C:19](I)[C:9]2[N:10]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)[CH:11]=[N:12][C:8]=2[CH:7]=1)=[O:5])[CH3:2].[C:22]([NH:25][C:26]1[CH:27]=[C:28](B(O)O)[CH:29]=[CH:30][CH:31]=1)(=[O:24])[CH3:23].C(O)CCO.C(=O)([O-])[O-].[K+].[K+]>C(COC)OC.O.Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1>[C:22]([NH:25][C:26]1[CH:31]=[C:30]([C:19]2[C:9]3[N:10]([C:13]4[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=4)[CH:11]=[N:12][C:8]=3[CH:7]=[C:6]([C:4]([O:3][CH2:1][CH3:2])=[O:5])[CH:20]=2)[CH:29]=[CH:28][CH:27]=1)(=[O:24])[CH3:23]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 104421,3-PropanediolHCID 11430Potassium CarbonateHCID 157274(3-Acetamidophenyl)boronic acidHCID 67485000HCID 67485000、化合物

生成物 1

HCID 11153793HCID 11153793、化合物

試薬・触媒・溶媒 3

HCID 178418476HCID 178418476、化合物触媒
HCID 962
Water
溶媒
HCID 80711,2-Dimethoxyethane溶媒

実験手順

A mixture of 5-ethoxycarbonyl-7-iodo-1-phenylbenzimidazole (0.70 g, 1.8 mmol), 3-acetamidophenylboronic acid (0.48 g, 2.7 mmol), 1,3-propanediol (0.65 ml, 8.9 mmol), potassium carbonate (1.23 g, 8.9 mmol) and bis(triphenylphosphin)palladium dichloride (50 mg, 0.07 mmol) in a mixture of dimethoxyethane (10 ml) and water (5 ml) was stirred at reflux for 1 hour. The cooled reaction mixture was concentrated under reduced pressure, and the concentrate was partitioned between water and ethyl acetate. The organic phase was dried and concentrated under reduced pressure, and the concentrate was triturated in ethyl acetate leaving the product as an off-white solid (0.48 g, 67%) m/z, 400.2 (M+H)+.

後処理

  1. temperatureat reflux for 1 hour
  2. customThe cooled reaction mixture
  3. concentrationwas concentrated under reduced pressure
  4. customthe concentrate was partitioned between water and ethyl acetate
  5. customThe organic phase was dried
  6. concentrationconcentrated under reduced pressure
  7. customthe concentrate was triturated in ethyl acetate leaving the product as an off-white solid (0.48 g, 67%) m/z, 400.2 (M+H)+

出典と根拠

ORDレコード
ord-936a8dcdaea648a9b4cf85ab86b66eae
出典データセット
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07700638B2

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