Ethyl trichloroacetate → N-methyl-4-(4-(2,2,2-trichloroacetamido)phenoxy)picolinamide

HRID 2094784

반응식

HRID 2094784 반응식
[NH2:1][C:2]1[CH:18]=[CH:17][C:5]([O:6][C:7]2[CH:12]=[CH:11][N:10]=[C:9]([C:13]([NH:15][CH3:16])=[O:14])[CH:8]=2)=[CH:4][CH:3]=1.C([O:21][C:22](=O)[C:23]([Cl:26])([Cl:25])[Cl:24])C>C1(C)C=CC=CC=1>[CH3:16][NH:15][C:13](=[O:14])[C:9]1[CH:8]=[C:7]([O:6][C:5]2[CH:17]=[CH:18][C:2]([NH:1][C:22](=[O:21])[C:23]([Cl:26])([Cl:25])[Cl:24])=[CH:3][CH:4]=2)[CH:12]=[CH:11][N:10]=1

참가 물질

4

반응물 2

HCID 10588Ethyl trichloroacetateHCID 166551294-(4-Aminophenoxy)-N-methylpicolinamide

생성물 1

HCID 68728447N-methyl-4-(4-(2,2,2-trichloroacetamido)phenoxy)picolinamide수율 87.6%

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
100 °C

실험 절차

4-(4-aminophenoxy)-N-methylpicolinamide (35 g, 0.144 mol) was mixed with ethyl-2,2,2-trichloroacetate (50 ml, 0.27 mol) in toluene (350 ml) at ambient temperature. The mixture was then heated to 100° C. under distillation mode for 2-3 hours. The organic solvent was degassed under reduced pressure to obtain oil. This oil was triturated with hexane (500 ml) to obtain (49 g) of the desired solid.

후처리

  1. customThe organic solvent was degassed under reduced pressure
  2. customto obtain oil
  3. customThis oil was triturated with hexane (500 ml)

출처 및 근거

ORD 기록
ord-284905d4c53f4ad3bcd9f9c896f6b010
출처 데이터셋
uspto-grants-2013_05
특허 번호
US08445687B2

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