HCID 66719111、化合物 → HCID 66823557、化合物

HRID 2362172ノート

反応式

HRID 2362172 の反応式
[C:1]([O:5][C:6](=[O:31])[NH:7][C:8]1([C:12]2[CH:17]=[CH:16][C:15]([C:18](=O)[C:19]([C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=3)=[CH:20]N(C)C)=[CH:14][CH:13]=2)[CH2:11][CH2:10][CH2:9]1)([CH3:4])([CH3:3])[CH3:2].[N:32]1[N:33]=[C:34]([NH2:38])[NH:35][C:36]=1[NH2:37]>C(O)(=O)C.C(O)C.C(Cl)Cl>[C:1]([O:5][C:6](=[O:31])[NH:7][C:8]1([C:12]2[CH:17]=[CH:16][C:15]([C:18]3[C:19]([C:24]4[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=4)=[CH:20][N:32]4[N:33]=[C:34]([NH2:38])[N:35]=[C:36]4[N:37]=3)=[CH:14][CH:13]=2)[CH2:11][CH2:10][CH2:9]1)([CH3:3])([CH3:2])[CH3:4]

参加物

6

反応物 2

HCID 66719111HCID 66719111、化合物HCID 178509197HCID 178509197、化合物

生成物 1

HCID 66823557HCID 66823557、化合物

試薬・触媒・溶媒 3

HCID 176Acetic Acid溶媒HCID 702Ethanol溶媒HCID 6344Dichloromethane溶媒

実験手順

A mixture of 1 (250 mg, 0.59 mmol) and 4H-[1,2,4]Triazole-3,5-diamine (58.91 mg, 0.59 mmol) in acetic acid (0.4 mL) and ethanol (1.6 mL) was heated under reflux for 6 hours. After cooling, the mixture was diluted with 15 mL of DCM, the combined organic phase was washed with NaHCO3 aq. and brine, dried over anhydrous Na2SO4 and concentrated. The residue was purified by prep.TLC to give 6-1. MS (ESI) m/e (M+H+) 457.3

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 6 hours
  3. temperatureAfter cooling
  4. washthe combined organic phase was washed with NaHCO3 aq. and brine
  5. dry with materialdried over anhydrous Na2SO4
  6. concentrationconcentrated
  7. customThe residue was purified by prep.TLC
  8. customto give 6-1

出典と根拠

ORDレコード
ord-24f6de24c67449ccb82af53f6132368b
出典データセット
uspto-grants-2014_04
特許番号
US08691825B2

反応ノート

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