Formaldehyde → 1-hydroxymethyl-3-cyano-4-trifluoromethyl-1H-pyrole

HRID 1983061ノート

反応式

HRID 1983061 の反応式
[C:1]([C:3]1[C:7]([C:8]([F:11])([F:10])[F:9])=[CH:6][NH:5][CH:4]=1)#[N:2].[O:12]1CCC[CH2:13]1.C=O.[OH-].C([N+](CCCC)(CCCC)CCCC)CCC>O>[OH:12][CH2:13][N:5]1[CH:6]=[C:7]([C:8]([F:11])([F:9])[F:10])[C:3]([C:1]#[N:2])=[CH:4]1

参加物

6

反応物 4

HCID 712FormaldehydeHCID 8028TetrahydrofuranHCID 2723671Tetrabutylammonium HydroxideHCID 151507031H-Pyrrole-3-carbonitrile, 4-(trifluoromethyl)-

生成物 1

HCID 231491381-hydroxymethyl-3-cyano-4-trifluoromethyl-1H-pyrole

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

585 mg of 3-cyano-4-trifluoromethyl-1H-pyrole, 10 ml of tetrahydrofuran and 10 ml of formaldehyde 36% in water were mixed. 0.1 ml of tetrabutylammonium hydroxide 10% in water was added to the mixture at room temperature, followed by stirring at room temperature for 30 minutes. The reaction mixture was poured into ice-water, and extracted with ethyl acetate. The organic layer was washed with saturated aqueous sodium chloride solution, dried over anhydrous magnesium sulfate, and filtered. The filtrate was concentrated under reduced pressure to obtain 1-hydroxymethyl-3-cyano-4-trifluoromethyl-1H-pyrole.

後処理

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed with saturated aqueous sodium chloride solution
  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-7f81b3411ec6426fa4c232b9c5d290af
出典データセット
uspto-grants-2009_06
特許番号
US07541374B2

反応ノート

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