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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
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Water → 2-[2-Chloro-4-(trifluoromethyl)phenoxy]-5-nitropyridine

HRID 2412524
ノート
印刷プレビュー

反応式

HRID 2412524 の反応式
C(=O)([O-])[O-].[Na+].[Na+].[Cl:7][C:8]1[CH:13]=[C:12]([C:14]([F:17])([F:16])[F:15])[CH:11]=[CH:10][C:9]=1[OH:18].Cl[C:20]1[CH:25]=[CH:24][C:23]([N+:26]([O-:28])=[O:27])=[CH:22][N:21]=1.O>CS(C)=O>[N+:26]([C:23]1[CH:22]=[N:21][C:20]([O:18][C:9]2[CH:10]=[CH:11][C:12]([C:14]([F:16])([F:17])[F:15])=[CH:13][C:8]=2[Cl:7])=[CH:25][CH:24]=1)([O-:28])=[O:27]
参加物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 962WaterHCID 10340Sodium CarbonateHCID 783082-Chloro-5-nitropyridineHCID 27366032-Chloro-4-(trifluoromethyl)phenol

生成物 1

HCID 133704682-[2-Chloro-4-(trifluoromethyl)phenoxy]-5-nitropyridine収率 81.9%

試薬・触媒・溶媒 1

HCID 679
Dimethyl Sulfoxide
溶媒
2 回

実験手順

7.6 g of anhydrous sodium carbonate and 9.8 g of 2-chloro-4-trifluoromethylphenol were added to 20 ml of dimethyl sulfoxide, and a solution having 7.9 g of 2-chloro-5-nitropyridine dissolved in 10 ml of dimethyl sulfoxide was added dropwise thereto at room temperature (i.e., about 20° to 30° C.) while stirring. After completion of the dropwise addition, the mixture was allowed to react at 50° C. for 30 minutes. After completion of the reaction, the reaction product was poured into water, followed by extracting with methylene chloride. The extracted phase was washed with water and dried, and the solvent was then distilled off to obtain 13 g of a crystal. The thus obtained crystal was recrystallized from n-hexane to obtain 9.8 g of a titled compound having a melting point of 69° to 72° C.

後処理

  1. additionwas added dropwise
  2. additionAfter completion of the dropwise addition
  3. customto react at 50° C. for 30 minutes
  4. customAfter completion of the reaction
  5. extractionby extracting with methylene chloride
  6. washThe extracted phase was washed with water
  7. customdried
  8. distillationthe solvent was then distilled off

出典と根拠

ORDレコード
ord-92b57840727442d98e8c66fe852aae4f
出典データセット
uspto-grants-1985_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04493730

反応ノート

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