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

HRID 2094784

反応式

HRID 2094784 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
100 °C

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-284905d4c53f4ad3bcd9f9c896f6b010
出典データセット
uspto-grants-2013_05
特許番号
US08445687B2

関連ノート

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