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

Tributylvinyltin → HCID 21188130、化合物

HRID 1383607
ノート
印刷プレビュー

反応式

HRID 1383607 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:5]=[C:4]([Cl:12])[C:3]=1[N:13]1[C:17]([CH3:18])=[C:16](I)[C:15]([CH3:20])=[N:14]1.[CH:21]([Sn](CCCC)(CCCC)CCCC)=[CH2:22]>CN(C)C=O.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[Cl:1][C:2]1[CH:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[CH:5]=[C:4]([Cl:12])[C:3]=1[N:13]1[C:17]([CH3:18])=[C:16]([CH:21]=[CH2:22])[C:15]([CH3:20])=[N:14]1
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

5

反応物 2

HCID 81998TributylvinyltinHCID 21188049HCID 21188049、化合物

生成物 1

HCID 21188130HCID 21188130、化合物

試薬・触媒・溶媒 2

HCID 178418397HCID 178418397、化合物触媒2 回HCID 6228Dimethylformamide溶媒

反応条件

温度
75 °C

実験手順

A solution of 1-(2,6-dichloro-4-trifluoromethylphenyl)-3,5-dimethyl4-iodopyrazole (1 g) in dimethylformamide (10 ml) containing yinyltri-n-butyltin (2 ml) and tetrakis(triphenylphosphine)palladium(0) (0.1 g) was stirred at 75° C. for 2 hours then left overnight at room temperature. The mixture was again heated at 75° C. for 2 hours then vinyltri-n-butyltin (2 ml) was added and the mixture heated at 75° C. for 2 hours. Tetrakis(triphenylphosphine)palladium(0) (0.1 g) was added and heating continued for a further 2 hours. The reaction mixture was evaporated and the residue partitioned between water and dichloromethane. The organic layer was separated, washed with water (×2), then brine, dried (Na2SO4) and evaporated. The residue was adsorbed onto silica gel (20 g) and purified by column chromatography on silica gel (150 g) eluted with hexane, then hexane with increasing amounts of dichloromethane and finally dichloromethane. Combination and evaporation of suitable fractions provided the title compound as yellow oil.

後処理

  1. waitthen left overnight at room temperature
  2. temperatureThe mixture was again heated at 75° C. for 2 hours
  3. temperaturethe mixture heated at 75° C. for 2 hours
  4. temperatureheating
  5. waitcontinued for a further 2 hours
  6. customThe reaction mixture was evaporated
  7. customthe residue partitioned between water and dichloromethane
  8. customThe organic layer was separated
  9. washwashed with water (×2)
  10. dry with materialbrine, dried (Na2SO4)
  11. customevaporated
  12. custompurified by column chromatography on silica gel (150 g)
  13. washeluted with hexane
  14. customCombination and evaporation of suitable fractions

出典と根拠

ORDレコード
ord-b4960cde2c5443c2839f90176e57d5a0
出典データセット
uspto-grants-2001_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06255333B1

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