Thionyl Chloride → 1-chloromethyl-3-cyano-4-trifluoromethyl-1H-pyrole

HRID 1983062노트

반응식

HRID 1983062 반응식
O[CH2:2][N:3]1[CH:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[C:5]([C:12]#[N:13])=[CH:4]1.S(Cl)([Cl:16])=O>C(Cl)(Cl)Cl>[Cl:16][CH2:2][N:3]1[CH:7]=[C:6]([C:8]([F:11])([F:10])[F:9])[C:5]([C:12]#[N:13])=[CH:4]1

참가 물질

4

반응물 2

HCID 24386Thionyl ChlorideHCID 231491381-hydroxymethyl-3-cyano-4-trifluoromethyl-1H-pyrole

생성물 1

HCID 231491561-chloromethyl-3-cyano-4-trifluoromethyl-1H-pyrole

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

The obtained 1-hydroxymethyl-3-cyano-4-trifluoromethyl-1H-pyrole was dissolved to 3 ml of chloroform, and 3 ml of thionyl chloride was added, followed by stirring at room temperature for 1 hour. After the reaction mixture was cooled to 0° C., it was poured into ice-water. The mixture was extracted with ethyl acetate. The organic layer was washed with saturated aqueous solution of sodium hydrogen carbonate, dried over anhydrous magnesium sulfate, and filtered. The filtrate was concentrated under reduced pressure to obtain 800 mg of 1-chloromethyl-3-cyano-4-trifluoromethyl-1H-pyrole.

후처리

  1. additionwas added
  2. temperatureAfter the reaction mixture was cooled to 0° C.
  3. extractionThe mixture was extracted with ethyl acetate
  4. washThe organic layer was washed with saturated aqueous solution of sodium hydrogen carbonate
  5. dry with materialdried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. concentrationThe filtrate was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-5f3391c69aca4f1d92ae41066add774a
출처 데이터셋
uspto-grants-2009_06
특허 번호
US07541374B2

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