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

Ethyl Acetate → HCID 178505686、化合物

HRID 1512164
ノート
印刷プレビュー

反応式

HRID 1512164 の反応式
Br[C:2]1[CH:20]=[CH:19][C:5]2[NH:6][C:7]([CH:9]=[CH:10][CH:11]3[CH2:16][CH2:15][C:14]([F:18])([F:17])[CH2:13][CH2:12]3)=[N:8][C:4]=2[CH:3]=1.[F:21][C:22]1[CH:27]=[CH:26][CH:25]=[C:24]([C:28]([F:31])([F:30])[F:29])[C:23]=1B(O)O.C(=O)([O-])[O-].[Na+].[Na+].C(OCC)(=O)C>C(COC)OC.[Pd](Cl)Cl.C(C1C=C[C-](P)C=1C(C)(C)C)(C)(C)C.[CH-]1C=CC=C1.[Fe+2].O>[F:17][C:14]1([F:18])[CH2:15][CH2:16][CH:11]([CH:10]=[CH:9][C:7]2[NH:6][C:5]3[CH:19]=[CH:20][C:2]([C:23]4[C:24]([C:28]([F:30])([F:31])[F:29])=[CH:25][CH:26]=[CH:27][C:22]=4[F:21])=[CH:3][C:4]=3[N:8]=2)[CH2:12][CH2:13]1
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 8857Ethyl AcetateHCID 10340Sodium CarbonateHCID 162171682-Fluoro-6-(trifluoromethyl)phenylboronic acidHCID 178506001HCID 178506001、化合物

生成物 1

HCID 178505686HCID 178505686、化合物

試薬・触媒・溶媒 3

HCID 131729813
Di-t-butyl-phosphinoferrocene palladium chloride
触媒
HCID 962Water溶媒
HCID 80711,2-Dimethoxyethane溶媒

実験手順

A solution of 5-bromo-2-[2-(4,4-difluoro-cyclohexyl)-vinyl]-1H-benzimidazole (0.030 g, 0.088 mmol, prepared as in STEP F above), 2-fluoro-6-trifluoromethylphenyl boronic acid (0.040 g, 0.19 mmol), 1,1-bis(di-t-butyl-phosphinoferrocene palladium chloride (0.012 g, 0.018 mmol) in dimethoxyethane (2 mL) and 2M sodium carbonate (1.0 mL, 2 mmol) was stirred at 95° C. for 18 h. The resulting solution was cooled to room temperature and poured into a solution of ethyl acetate and water (1:1, 50 mL). The layers were separated. The organic layer was washed with brine, dried over sodium sulfate, filtered and concentrated. The residue was purified on silica using ethyl acetate/hexanes 3:7 as eluent to yield 2-[2-(4,4-difluoro-cyclohexyl)-vinyl]-5-(2-fluoro-6-trifluoromethyl-phenyl)-1H-benzimidazole.

後処理

  1. customThe layers were separated
  2. washThe organic layer was washed with brine
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe residue was purified on silica

出典と根拠

ORDレコード
ord-c23cb18f734d479bb366fb41ea118daa
出典データセット
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08217060B2

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