Stannous chloride dihydrate → HCID 10967548、化合物

HRID 377500ノート

反応式

HRID 377500 の反応式
[N:1]1([C:6]2[N:11]=[C:10]([N:12]3[CH:16]=[CH:15][N:14]=[CH:13]3)[C:9]([N+:17]([O-])=O)=[C:8]([CH:20]([CH3:22])[CH3:21])[N:7]=2)[CH:5]=[CH:4][N:3]=[CH:2]1.O.O.[Sn](Cl)Cl>C(O)C>[N:1]1([C:6]2[N:11]=[C:10]([N:12]3[CH:16]=[CH:15][N:14]=[CH:13]3)[C:9]([NH2:17])=[C:8]([CH:20]([CH3:22])[CH3:21])[N:7]=2)[CH:5]=[CH:4][N:3]=[CH:2]1

参加物

4

反応物 2

HCID 61436Stannous chloride dihydrateHCID 53792902HCID 53792902、化合物

生成物 1

HCID 10967548HCID 10967548、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Dissolve 2,4-bis(1H-imidazol-1-yl)-5-nitro-6-(2-propyl)pyrimidine (16 g, 53.5 mmol) in 300 mL of ethanol and add 35 g of tin (II) chloride dihydrate. Stir for 2 hours at ambient temperature. Remove the solvent under vacuum and slurry the residue in 2 L of CH2Cl2. Wash with 2×3 L 10% KOH. Dry the CH2Cl2 portion over MgSO4, treat with charcoal, filter, and concentrate the filtrate under vacuum. Crystallize the residue from ethyl acetate to provide 2,4-bis(1H-imidazol-1-yl)-6-(2-propyl)pyrimidin-5-amine.

後処理

  1. customRemove the solvent under vacuum
  2. washWash with 2×3 L 10% KOH
  3. dry with materialDry the CH2Cl2 portion over MgSO4
  4. additiontreat with charcoal
  5. filtrationfilter
  6. concentrationconcentrate the filtrate under vacuum
  7. customCrystallize the residue from ethyl acetate

出典と根拠

ORDレコード
ord-c14fb4bc005b4880828a8b1c25e04c88
出典データセット
uspto-grants-2000_02
特許番号
US06025489

反応ノート

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