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

Benzyl Bromide → Benzyl 5-cyano-2-(trifluoromethyl)benzoate

HRID 889531
ノート
印刷プレビュー

反応式

HRID 889531 の反応式
Cl[C:2]1[CH:3]=[CH:4][C:5]([C:11]([F:14])([F:13])[F:12])=[C:6]([CH:10]=1)[C:7]([OH:9])=[O:8].C(=O)([O-])[O-].[Cs+].[Cs+].[CH2:21](Br)[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1.C[C:30]([N:32](C)C)=O>[C-]#N.[Zn+2].[C-]#N.[Zn].C(P([Pd]P(C(C)(C)C)(C(C)(C)C)C(C)(C)C)(C(C)(C)C)C(C)(C)C)(C)(C)C>[C:30]([C:2]1[CH:3]=[CH:4][C:5]([C:11]([F:14])([F:13])[F:12])=[C:6]([CH:10]=1)[C:7]([O:9][CH2:21][C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1)=[O:8])#[N:32]
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

8

反応物 4

HCID 7498Benzyl BromideHCID 10796Cesium carbonateHCID 31374DimethylacetamideHCID 27738595-Chloro-2-(trifluoromethyl)benzoic acid

生成物 1

HCID 67970345Benzyl 5-cyano-2-(trifluoromethyl)benzoate収率 57%

試薬・触媒・溶媒 3

HCID 11186
Zinc cyanide (Zn(CN)2)
触媒
HCID 23994Zinc触媒
HCID 178454917HCID 178454917、化合物触媒

反応条件

温度
95 °C

実験手順

Under a nitrogen atmosphere, to a solution of 5-chloro-2-(trifluoromethyl)benzoic acid (5.02 g, 22.35 mmol, 1.0 equiv) in DMA (45 mL), add zinc(II) cyanide (1.77 g, 15.07 mmol, 0.67 equiv), zinc dust (<10 μM, 330 mg, 5.05 mmol, 0.23 equiv), and bis(tri-tert-butylphosphino)palladium (540 mg, 1.06 mmol, 0.05 equiv). Stir the mixture under a nitrogen atmosphere at 95° C. for 9.5 hours. Add cesium carbonate (13.3 g, 40.82 mmol, 1.83 equiv), then benzyl bromide (3.0 mL, 25.15 mmol, 1.13 equiv), and stir under air at room temperature for 3.5 hours. Concentrate under reduced pressure, add water, and extract with EtOAc. Separate the organic phase and wash with saturated aqueous NaCl, dry over MgSO4, filter, and concentrate under reduced pressure. Subject the resulting crude material to flash chromatography on silica gel eluting with a 0-50% EtOAc/hexanes gradient to give the title compound (3.9 g, 57%). MS (m/z) 306 (M+1).

後処理

  1. concentrationConcentrate under reduced pressure
  2. additionadd water
  3. extractionextract with EtOAc
  4. customSeparate the organic phase
  5. washwash with saturated aqueous NaCl
  6. dry with materialdry over MgSO4
  7. filtrationfilter
  8. concentrationconcentrate under reduced pressure

出典と根拠

ORDレコード
ord-060b2d212a454d7caae7414001d59693
出典データセット
uspto-grants-2012_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08252831B2

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