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Hydrochloric Acid → Pyrithiobac

HRID 2106966
ノート
印刷プレビュー

反応式

HRID 2106966 の反応式
Cl.N[C:3]1[CH:11]=[CH:10][CH:9]=[C:8]([Cl:12])[C:4]=1[C:5]([OH:7])=[O:6].Cl.[CH3:14][O:15][C:16]1[CH:21]=[C:20]([O:22][CH3:23])[N:19]=[C:18]([SH:24])[N:17]=1.[OH-].[Na+]>O>[Cl:12][C:8]1[CH:9]=[CH:10][CH:11]=[C:3]([S:24][C:18]2[N:17]=[C:16]([O:15][CH3:14])[CH:21]=[C:20]([O:22][CH3:23])[N:19]=2)[C:4]=1[C:5]([OH:7])=[O:6]
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 313Hydrochloric Acid2 回HCID 14798Sodium HydroxideHCID 53444447HCID 53444447、化合物HCID 178493561HCID 178493561、化合物

生成物 1

HCID 91781Pyrithiobac収率 22.9%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

5.0 g of 2-amino-6-chlorobenzoic acid hydrochloride was converted to a diazonium salt with 2.3 g of sodium nitride and concentrated hydrochloric acid. Then, this diazonium salt was gradually dropwise added to a solution comprising 4.8 g of 4,6-dimethoxy-2-mercaptopyrimidine, 2.4 g of sodium hydroxide and 40 ml of water at 0° C. After completion of the dropwise addition, the mixture was stirred at room temperature for 2 hours to complete the reaction. Concentrated hydrochloric acid was added to the reaction solution, and then, the mixture was extracted with ethyl acetate. The extract was dried, and then the solvent was distilled off under reduced pressure. The residue thereby obtained was purified by column chromatography to obtain 1.8 g of the desired compound as ocher powder.

後処理

  1. customat 0° C
  2. additionAfter completion of the dropwise addition
  3. customthe reaction
  4. extractionthe mixture was extracted with ethyl acetate
  5. customThe extract was dried
  6. distillationthe solvent was distilled off under reduced pressure
  7. customThe residue thereby obtained
  8. customwas purified by column chromatography

出典と根拠

ORDレコード
ord-ad6f34de46ba4188a8fdee6e9555420b
出典データセット
uspto-grants-1990_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04932999

反応ノート

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