Trichloroacetonitrile → 3-{4-[2,4-bis(trichloromethyl)-s-triazine-6-yl]phenyl thio}propionic Acid

HRID 1748913

반응식

HRID 1748913 반응식
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([S:9][CH2:10][CH2:11][C:12]([OH:14])=[O:13])=[CH:5][CH:4]=1)#[N:2].[Br-].[Br-].[Br-].[Al+3].[Cl:19][C:20]([Cl:24])([Cl:23])[C:21]#[N:22]>>[Cl:19][C:20]([Cl:24])([Cl:23])[C:21]1[N:22]=[C:21]([C:20]([Cl:24])([Cl:23])[Cl:19])[N:22]=[C:1]([C:3]2[CH:4]=[CH:5][C:6]([S:9][CH2:10][CH2:11][C:12]([OH:14])=[O:13])=[CH:7][CH:8]=2)[N:2]=1

참가 물질

4

반응물 3

HCID 11011TrichloroacetonitrileHCID 166749BromhydrolHCID 226666023-[(4-Cyanophenyl)sulfanyl]propanoic acid

생성물 1

HCID 601112433-{4-[2,4-bis(trichloromethyl)-s-triazine-6-yl]phenyl thio}propionic Acid

실험 절차

A solution containing 22 g of 3-(4-cyanophenylthio) propionic acid (106 mmol) and 2 g of aluminum tribromide (AlBr3) in 150 g of trichloroacetonitrile was dried at room temperature and bubbled with HCl. The solution was heated with a heat-gun in order to dissolve the starting materials remaining undissolved. The process of reaction was checked by TLC. The reaction product was formed gradually with the lapse of time. Then, the reaction was quenched after 24 hours and the reaction mixture was extracted with 1000 mL of diethyl ether. The resultant product was washed with deionized water and dried over anhydrous magnesium sulfate.

후처리

  1. customwas dried at room temperature
  2. custombubbled with HCl
  3. temperatureThe solution was heated with
  4. temperaturea heat-gun in order
  5. dissolutionto dissolve the starting materials
  6. customThe process of reaction
  7. customThe reaction product was formed gradually with the lapse of time
  8. customThen, the reaction was quenched after 24 hours
  9. extractionthe reaction mixture was extracted with 1000 mL of diethyl ether
  10. washThe resultant product was washed with deionized water
  11. dry with materialdried over anhydrous magnesium sulfate

출처 및 근거

ORD 기록
ord-57398dd6e6574f238fac197d343ea13c
출처 데이터셋
uspto-grants-2015_10
특허 번호
US09152041B2

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