2-Chloro-1,1-diethoxyethane → Thiazole, 2-[(3,4,4-trifluoro-3-butenyl)thio]-

HRID 1793116

반응식

HRID 1793116 반응식
[C:1](=[S:11])([S:3][CH2:4][CH2:5][C:6]([F:10])=[C:7]([F:9])[F:8])[NH2:2].[CH2:12](OC(OCC)CCl)[CH3:13].O.C1(C)C=CC(S(O)(=O)=O)=CC=1>C(O)(=O)C>[F:10][C:6](=[C:7]([F:9])[F:8])[CH2:5][CH2:4][S:3][C:1]1[S:11][CH:12]=[CH:13][N:2]=1

참가 물질

5

반응물 3

HCID 121282-Chloro-1,1-diethoxyethaneHCID 521998p-Toluenesulfonic acid monohydrateHCID 112985983,4,4-Trifluoro-3-butenyl dithiocarbamate

생성물 1

HCID 11447455Thiazole, 2-[(3,4,4-trifluoro-3-butenyl)thio]-

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
95 °C

실험 절차

3 g (14.9 mmol) of 3,4,4-trifluoro-3-butenyl dithiocarbamate in 15 ml of glacial acetic acid are admixed with 2.3 g (15.1 mmol) of chloroacetaldehyde diethyl acetal and 40 mg of p-toluenesulphonic acid monohydrate. The mixture is stirred at 95° C. for 1.5 h and, after cooling to room temperature, is then concentrated by evaporation under reduced pressure. The evaporation residue is taken up in dichloromethane and washed with 1 N sodium hydroxide solution, and the organic phase is removed, dried over Na2SO4 and concentrated by evaporation under reduced pressure. 2.8 g (81.5% of theory; purity by GC/MS: 97.7 area %) of an oil are obtained.

후처리

  1. temperatureafter cooling to room temperature
  2. concentrationis then concentrated by evaporation under reduced pressure
  3. washwashed with 1 N sodium hydroxide solution
  4. customthe organic phase is removed
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated by evaporation under reduced pressure
  7. custom2.8 g (81.5% of theory; purity by GC/MS: 97.7 area %) of an oil are obtained

출처 및 근거

ORD 기록
ord-ee4b179577564cf2a3db73ccda4e6fac
출처 데이터셋
uspto-grants-2006_07
특허 번호
US07078527B2

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