Water → HCID 178484578、化合物

HRID 931189ノート

反応式

HRID 931189 の反応式
[NH2:1][C:2]1[N:7]=[C:6]([N:8]2[CH2:13][CH2:12][CH2:11][C@@H:10]([C:14]([N:16]([CH3:18])[CH3:17])=[O:15])[CH2:9]2)[CH:5]=[CH:4][C:3]=1[N+:19]([O-])=O.[F:22][CH:23]([F:33])[O:24][C:25]1[CH:26]=[C:27]([CH:30]=[CH:31][CH:32]=1)[CH:28]=O.O.S(S([O-])=O)([O-])=O.[Na+].[Na+]>CN(C)C=O>[F:22][CH:23]([F:33])[O:24][C:25]1[CH:26]=[C:27]([C:28]2[NH:1][C:2]3=[N:7][C:6]([N:8]4[CH2:13][CH2:12][CH2:11][C@@H:10]([C:14]([N:16]([CH3:18])[CH3:17])=[O:15])[CH2:9]4)=[CH:5][CH:4]=[C:3]3[N:19]=2)[CH:30]=[CH:31][CH:32]=1

参加物

6

反応物 4

HCID 962WaterHCID 24489Sodium DithioniteHCID 27369853-(Difluoromethoxy)benzaldehydeHCID 117966493(R)-1-(6-amino-5-nitropyridin-2-yl)-N,N-dimethylpiperidine-3-carboxamide

生成物 1

HCID 178484578HCID 178484578、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

反応条件

温度
110 °C

実験手順

Into a 4 mL vial was added (R)-1-(6-amino-5-nitropyridin-2-yl)-N,N-dimethylpiperidine-3-carboxamide (500 μL, 0.3M) dissolved in N,N-dimethylformamide followed by 3-(difluoromethoxy)benzaldehyde (950 μL, 0.158M) dissolved in N,N-dimethylformamide. Water (50 μL) was added followed by sodium hydrosulfite (574 μmol) under a nitrogen atmosphere. The vial was capped and shaken at 110° C. for 18 h. The solvent was removed by Speedvac and the residue was purified by HPLC to afford the title compound. MS (API-ES+) (M+H) 416.2; HPLC retention time 1.392 min (Method E).

後処理

  1. customThe vial was capped
  2. customThe solvent was removed by Speedvac
  3. customthe residue was purified by HPLC

出典と根拠

ORDレコード
ord-c5c7fde5f03248d9b72f1696363a3fad
出典データセット
uspto-grants-2016_03
特許番号
US09296745B2

反応ノート

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