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

HRID 1983061노트

반응식

HRID 1983061 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7f81b3411ec6426fa4c232b9c5d290af
출처 데이터셋
uspto-grants-2009_06
특허 번호
US07541374B2

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