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 Carbonate → HCID 57969705、化合物

HRID 384059
ノート
印刷プレビュー

反応式

HRID 384059 の反応式
CC1(C)C(C)(C)OB([C:9]2[CH:14]=[CH:13][N:12]=[C:11]3[N:15]([C:18]([C:31]4[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=4)([C:25]4[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=4)[C:19]4[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=4)[N:16]=[CH:17][C:10]=23)O1.Br[C:39]1[CH:40]=[C:41]([C:45]([CH3:50])([CH2:48][CH3:49])[C:46]#[N:47])[CH:42]=[CH:43][CH:44]=1.C(=O)([O-])[O-].[Na+].[Na+]>O1CCOCC1.CC(C)([P](C(C)(C)C)([Pd][P](C(C)(C)C)(C(C)(C)C)C(C)(C)C)C(C)(C)C)C>[CH3:50][C:45]([C:41]1[CH:40]=[CH:39][CH:44]=[C:43]([C:9]2[CH:14]=[CH:13][N:12]=[C:11]3[N:15]([C:18]([C:19]4[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=4)([C:25]4[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=4)[C:31]4[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=4)[N:16]=[CH:17][C:10]=23)[CH:42]=1)([CH2:48][CH3:49])[C:46]#[N:47]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 10340Sodium CarbonateHCID 579696322-(3-Bromophenyl)-2-methylbutanenitrileHCID 57969821HCID 57969821、化合物

生成物 1

HCID 57969705HCID 57969705、化合物収率 59%

試薬・触媒・溶媒 2

HCID 178418851HCID 178418851、化合物触媒
HCID 31275
1,4-Dioxane
溶媒

実験手順

A suspension of 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-1-trityl-1H-pyrazolo[3,4-b]pyridine (307 mg, 0.630 mmol), 2-(3-bromophenyl)-2-methylbutanenitrile (150 mg, 0.630 mmol) and 2 M aqueous solution of sodium carbonate (0.945 ml, 1.89 mmol) in dioxane (4 ml) was degassed by vacuum/nitrogen cycles (×5). Bis(tri-tert-butylphosphine)palladium(0) (16.10 mg, 0.032 mmol) was added and the resultant mixture was degassed by vacuum/nitrogen cycles (×5) and stirred at room temperature for 18 hours. The mixture was partitioned between ethyl acetate and a saturated aqueous solution of sodium carbonate. The organic phase was dried over magnesium sulfate, filtered and concentrated in vacuo. The residue was purified on silica gel by flash column chromatography to afford the title compound as a sticky white solid (0.240 mg, 80% purity, 59% yield).

後処理

  1. customwas degassed by vacuum/nitrogen cycles (×5)
  2. customthe resultant mixture was degassed by vacuum/nitrogen cycles (×5)
  3. customThe mixture was partitioned between ethyl acetate
  4. dry with materialThe organic phase was dried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customThe residue was purified on silica gel by flash column chromatography

出典と根拠

ORDレコード
ord-7237cdf29058401691e411f524451d43
出典データセット
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08367697B2

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