Sodium hydride → Pyrithiobac sodium

HRID 2106968ノート

反応式

HRID 2106968 の反応式
[Cl:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]([S:11][C:12]2[N:17]=[C:16]([O:18][CH3:19])[CH:15]=[C:14]([O:20][CH3:21])[N:13]=2)[C:3]=1[C:4]([OH:6])=[O:5].[H-].[Na+:23]>O1CCCC1>[Cl:1][C:2]1[CH:10]=[CH:9][CH:8]=[C:7]([S:11][C:12]2[N:13]=[C:14]([O:20][CH3:21])[CH:15]=[C:16]([O:18][CH3:19])[N:17]=2)[C:3]=1[C:4]([O-:6])=[O:5].[Na+:23]

参加物

4

反応物 2

HCID 24758Sodium hydrideHCID 91781Pyrithiobac

生成物 1

HCID 23682187Pyrithiobac sodium収率 99.2%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

1.7 g of 2-chloro-6-[(4,6-dimethoxy-2-pyrimidinyl)thio]benzoic acid dissolved in 10 ml of tetrahydrofuran was gradually dropwise added to a suspension of 0.2 g of 60% sodium hydride in 20 ml of tetrahydrofuran. The mixture was reacted under stirring for 30 minutes. After completion of the reaction, the solvent was distilled off under reduced pressure. Isopropyl ether was added to the residue, and a solid was collected by filtration. The solid was dried to obtain 1.8 g of the desired compound as white powder.

後処理

  1. customThe mixture was reacted
  2. customAfter completion of the reaction
  3. distillationthe solvent was distilled off under reduced pressure
  4. additionIsopropyl ether was added to the residue
  5. filtrationa solid was collected by filtration
  6. customThe solid was dried

出典と根拠

ORDレコード
ord-7b5cb9a5e4b74c30923f2fcee7b95e46
出典データセット
uspto-grants-1990_06
特許番号
US04932999

反応ノート

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