Acetic Acid → HCID 69043799、化合物

HRID 77735ノート

反応式

HRID 77735 の反応式
[CH3:1][C:2]1[N:7]=[CH:6][C:5]([NH:8][C:9](=[O:20])[C:10]2[CH:15]=[CH:14][CH:13]=[C:12]([C:16]([F:19])([F:18])[F:17])[CH:11]=2)=[CH:4][C:3]=1[C:21]1[CH:26]=[CH:25][CH:24]=[C:23]([N+:27]([O-])=O)[CH:22]=1.C(O)(=O)C.C([O-])([O-])=O.[Na+].[Na+]>C(O)C.[Fe]>[NH2:27][C:23]1[CH:22]=[C:21]([C:3]2[CH:4]=[C:5]([NH:8][C:9](=[O:20])[C:10]3[CH:15]=[CH:14][CH:13]=[C:12]([C:16]([F:19])([F:17])[F:18])[CH:11]=3)[CH:6]=[N:7][C:2]=2[CH3:1])[CH:26]=[CH:25][CH:24]=1

参加物

6

反応物 3

HCID 176Acetic AcidHCID 10340Sodium CarbonateHCID 69043081HCID 69043081、化合物

生成物 1

HCID 69043799HCID 69043799、化合物

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 702Ethanol溶媒

反応条件

温度
87 °C

実験手順

To a solution of N-[6-methyl-5-(3-nitrophenyl)pyridin-3-yl]-3-(trifluoromethyl)benzamide (0.150 g, 0.000374 mol) in ethanol (3 mL) was added acetic acid (0.5 mL, 0.009 mol) and iron powder (0.11 g, 0.0020 mol). The reaction was heated at 87° C. for 2 hours. It was then neutralized with Na2CO3 and extracted with EtOAc and the organic extracts were washed with water, saturated NaCl, dried (MgSO4) and stripped in vacuo. The residue was used in the next reaction without purification. MS (ES) (M+H)=372.

後処理

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

出典と根拠

ORDレコード
ord-eee8222bdaa24ddfa139b5247e6b63ab
出典データセット
uspto-grants-2014_09
特許番号
US08841318B2

反応ノート

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