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

Potassium Iodide → 6-Trifluoromethylsulphonyl-2,2-dimethyl-2H-benzo(b)pyran

HRID 1086316
ノート
印刷プレビュー

反応式

HRID 1086316 の反応式
[F:1][C:2]([F:14])([F:13])[S:3]([C:6]1[CH:11]=[CH:10][C:9]([OH:12])=[CH:8][CH:7]=1)(=[O:5])=[O:4].C(=O)([O-])[O-].[K+].[K+].[I-].[K+].Cl[C:24]([CH3:28])([CH3:27])[C:25]#[CH:26]>CC(=O)CC>[F:14][C:2]([F:13])([F:1])[S:3]([C:6]1[CH:7]=[CH:8][C:9]2[O:12][C:24]([CH3:28])([CH3:27])[CH:25]=[CH:26][C:10]=2[CH:11]=1)(=[O:4])=[O:5]
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

6

反応物 4

HCID 4875Potassium Iodide2 回HCID 11430Potassium Carbonate2 回HCID 706791-Butyne, 3-chloro-3-methyl-2 回HCID 148574264-Trifluoromethanesulfonylphenol

生成物 1

HCID 148574316-Trifluoromethylsulphonyl-2,2-dimethyl-2H-benzo(b)pyran収率 38.9%

試薬・触媒・溶媒 1

HCID 6569
Methyl Ethyl Ketone
溶媒

反応条件

温度
180 °C

実験手順

1 g (4.4 mmol) of 4-trifluoromethylsulphonylphenol are stirred under argon at 80°-90° C. for 20 hours together with 0.66 g of potassium carbonate, 80 mg of potassium iodide and 2 g of 3-chloro-3-methyl-1-butyne in 13 ml of dry butanone. 0.33 g of potassium carbonate, 40 mg of potassium iodide and 1 g of 3-chloro-3-methyl-1-butyne are then added once again and the mixture is stirred at 80°-90° C. for a further 20 hours. It is then allowed to cool and is filtered, and the filtrate is evaporated. The residue is taken up in 20 ml of methylene chloride, washed with water (2×20 ml), dried and evaporated. The oil which remains (1.3 g) is heated under argon to 180° C. for 3 hours in o-dichlorobenzene (3 ml). After distilling off the solvent, the residue is chromatographed on silica gel. 0.5 g of colorless oil are obtained (50 % of theory). M+ =292 (5).

後処理

  1. temperatureto cool
  2. filtrationis filtered
  3. customthe filtrate is evaporated
  4. washwashed with water (2×20 ml)
  5. customdried
  6. customevaporated
  7. distillationAfter distilling off the solvent
  8. customthe residue is chromatographed on silica gel

出典と根拠

ORDレコード
ord-18eb613b8aa445dbbbb1df7cf5be1768
出典データセット
uspto-grants-1991_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05028711

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