Triethylamine → N-(5-iodo-6-methylpyridin-3-yl)-3-(trifluoromethyl)benzamide

HRID 1894905ノート

反応式

HRID 1894905 の反応式
[I:1][C:2]1[CH:3]=[C:4]([NH2:9])[CH:5]=[N:6][C:7]=1[CH3:8].C(N(CC)CC)C.[F:17][C:18]([F:29])([F:28])[C:19]1[CH:20]=[C:21]([CH:25]=[CH:26][CH:27]=1)[C:22](Cl)=[O:23]>C(Cl)Cl>[I:1][C:2]1[CH:3]=[C:4]([NH:9][C:22](=[O:23])[C:21]2[CH:25]=[CH:26][CH:27]=[C:19]([C:18]([F:17])([F:28])[F:29])[CH:20]=2)[CH:5]=[N:6][C:7]=1[CH3:8]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 752573-(Trifluoromethyl)benzoyl chlorideHCID 591982915-Iodo-6-methylpyridin-3-amine

生成物 1

HCID 69042846N-(5-iodo-6-methylpyridin-3-yl)-3-(trifluoromethyl)benzamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

To a solution of 5-iodo-6-methylpyridin-3-amine (125 mg, 0.534 mmol) in methylene chloride (1 mL) was added triethylamine (0.087 mL, 0.627 mmol) and cooled at 0° C. Into the reaction was added 3-(trifluoromethyl)benzoyl chloride (0.0812 mL, 0.538 mmol) dropwise and stirred at 0° C. for 45 minutes and at 25° C. for 16 hours. The reaction was extracted with EtOAc and the organic extracts were washed with water saturated Na2CO3, saturated NaCl, dried (MgSO4) and stripped in vacuo. The product was used in the next reaction without purification.

後処理

  1. extractionThe reaction was extracted with EtOAc
  2. washthe organic extracts were washed with water saturated Na2CO3, saturated NaCl
  3. dry with materialdried (MgSO4)
  4. customThe product was used in the next reaction without purification

出典と根拠

ORDレコード
ord-fdd556997cbd490fa4e181c61ae4a092
出典データセット
uspto-grants-2013_08
特許番号
US08513270B2

反応ノート

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