Formaldehyde → HCID 23149182、化合物

HRID 1983055ノート

反応式

HRID 1983055 の反応式
[Cl:1][C:2]([Cl:10])([F:9])[S:3][C:4]1[CH:5]=[N:6][NH:7][CH:8]=1.[O:11]1CCC[CH2:12]1.C=O>O.[OH-].C([N+](CCCC)(CCCC)CCCC)CCC>[Cl:1][C:2]([Cl:10])([F:9])[S:3][C:4]1[CH:5]=[N:6][N:7]([CH2:12][OH:11])[CH:8]=1

参加物

6

反応物 3

HCID 712FormaldehydeHCID 8028TetrahydrofuranHCID 23149183HCID 23149183、化合物

生成物 1

HCID 23149182HCID 23149182、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒3 回HCID 2723671Tetrabutylammonium Hydroxide溶媒

実験手順

0.19 g of 4-{[dichlorofluoromethyl]thio}-1H-pyrazole was dissolved to 5 ml of tetrahydrofuran. 5 ml of formaldehyde 36% in water and 0.1 ml of tetrabutylammonium hydroxide 10% in water were added to the solution, followed by stirring at room temperature for 4 hours. Water was added to the reaction mixture, and extracted with MTBE. The organic layer was washed with water, dried over anhydrous magnesium sulfate, and filtered. The filtrate was concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to obtain 0.22 g of 4-{[dichlorofluoromethyl]thio}-1H-pyrazole-1-ylmethanol.

後処理

  1. extractionextracted with MTBE
  2. washThe organic layer was washed with water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. concentrationThe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-88e67316c6b842e086de44ac8c9843c5
出典データセット
uspto-grants-2009_06
特許番号
US07541374B2

反応ノート

読み込み中…