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

Ammonium Chloride → 4-Ethinyl-1,5-dimethyl-3-(trifluoromethyl)-1h-pyrazole

HRID 971086
ノート
印刷プレビュー

反応式

HRID 971086 の反応式
Cl[CH:2]=[CH:3][C:4]1[C:5]([C:11]([F:14])([F:13])[F:12])=[N:6][N:7]([CH3:10])[C:8]=1[CH3:9].CC(C)([O-])C.[K+].[Cl-].[NH4+]>C1COCC1>[C:3]([C:4]1[C:5]([C:11]([F:13])([F:14])[F:12])=[N:6][N:7]([CH3:10])[C:8]=1[CH3:9])#[CH:2]
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 3

HCID 25517Ammonium ChlorideHCID 23665647Potassium tert-butoxideHCID 851512404-(2-chloroethenyl)-1,5-dimethyl-3-(trifluoromethyl)-1H-pyrazole

生成物 1

HCID 104424634-Ethinyl-1,5-dimethyl-3-(trifluoromethyl)-1h-pyrazole収率 79%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
0 °C

実験手順

1.27 g (5.67 mmol) of 4-(2-chloroethenyl)-1,5-dimethyl-3-(trifluoromethyl)-1H-pyrazole from Example 1 are dissolved in 40 ml of dry THF and placed under a protective gas atmosphere. After cooling the reaction solution to 0° C., 1.91 (17.0 mmol) of potassium tert-butoxide are introduced and, after the addition is complete, the mixture is stirred at 20° C. for 3 hours. After the end of the reaction, a saturated ammonium chloride solution (25 ml) is added and the mixture is extracted twice with 30 ml each time of methylene chloride. The combined organic phases are dried over magnesium sulphate, the solvent is removed by distillation and 4-ethynyl-1,5-dimethyl-3-(trifluoromethyl)-1H-pyrazole is isolated as a microcrystalline solid in a yield of 79% of theory.

後処理

  1. additionafter the addition
  2. customAfter the end of the reaction
  3. extractionthe mixture is extracted twice with 30 ml each time of methylene chloride
  4. dry with materialThe combined organic phases are dried over magnesium sulphate
  5. customthe solvent is removed by distillation

出典と根拠

ORDレコード
ord-39a38832c0b64342b84735591a9537eb
出典データセット
uspto-grants-2007_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07312350B2

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