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Acetic Acid → 2-[3-(difluoromethyl)-5-methyl-1-(tetrahydro-2H-pyran-2-yl)-1H-pyrazol-4-yl]imidazo[4,5-d]dipyrido[2,3-b: 4',3'-f]azepin-3(8H)-ol

HRID 75220
ノート
印刷プレビュー

反応式

HRID 75220 の反応式
[N:1]1[C:6]2[NH:7][C:8]3[CH:18]=[N:17][CH:16]=[CH:15][C:9]=3/[C:10](=[N:13]/[OH:14])/[C:11](=O)[C:5]=2[CH:4]=[CH:3][CH:2]=1.C([O-])(=O)C.[NH4+:23].[F:24][CH:25]([F:40])[C:26]1[C:30]([CH:31]=O)=[C:29]([CH3:33])[N:28]([CH:34]2[CH2:39][CH2:38][CH2:37][CH2:36][O:35]2)[N:27]=1.C(O)(=O)C>>[F:24][CH:25]([F:40])[C:26]1[C:30]([C:31]2[N:13]([OH:14])[C:10]3[C:9]4[CH:15]=[CH:16][N:17]=[CH:18][C:8]=4[NH:7][C:6]4[N:1]=[CH:2][CH:3]=[CH:4][C:5]=4[C:11]=3[N:23]=2)=[C:29]([CH3:33])[N:28]([CH:34]2[CH2:39][CH2:38][CH2:37][CH2:36][O:35]2)[N:27]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 4

HCID 176Acetic AcidHCID 517165Ammonium AcetateHCID 866132733-(difluoromethyl)-5-methyl-1-(tetrahydro-2H-pyran-2-yl)-1H-pyrazole-4-carbaldehydeHCID 178516816HCID 178516816、化合物

生成物 1

HCID 668871612-[3-(difluoromethyl)-5-methyl-1-(tetrahydro-2H-pyran-2-yl)-1H-pyrazol-4-yl]imidazo[4,5-d]dipyrido[2,3-b: 4',3'-f]azepin-3(8H)-ol

反応条件

温度
80 °C

実験手順

A mixture of (6Z)-5H-dipyrido[2,3-b:4′,3′-f]azepine-5,6(11H)-dione 6-oxime (1.00 g, 4.16 mmol), ammonium acetate (6.00 g, 77.8 mmol) and 3-(difluoromethyl)-5-methyl-1-(tetrahydro-2H-pyran-2-yl)-1H-pyrazole-4-carbaldehyde (2.50 g, 8.19 mmol) in acetic acid (6.0 mL, 0.106 mol) was stirred at 80° C. for 2 h. The reaction was partitioned between dichloromethane/isopropanol (5:1) and water and the organic extract was washed with NaHCO3, brine, dried (MgSO4) and concentrated in vacuo. The residue was used in the next reaction without purification. Mass spec: (EI) m/z=466 (M+1).

後処理

  1. customThe reaction was partitioned between dichloromethane/isopropanol (5:1) and water
  2. extractionthe organic extract
  3. washwas washed with NaHCO3, brine
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated in vacuo
  6. customThe residue was used in the next reaction without purification

出典と根拠

ORDレコード
ord-85aec97017a7463cbd169e154813a481
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08835423B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート