N-(4-Ethoxy-5-methylcarbamoylpyridin-2-ylmethyl)-N'-(fluoren-9-ylmethyloxycarbonyl)thiourea → 9H-Fluoren-9-ylmethyl (7-ethoxy-6-methylcarbamoyl-2H-imidazo[1,5-a]pyridin-3-ylidene)carbamate

HRID 249729

反応式

HRID 249729 の反応式
[CH2:1]([O:3][C:4]1[C:9]([C:10](=[O:13])[NH:11][CH3:12])=[CH:8][N:7]=[C:6]([CH2:14][NH:15][C:16]([NH:18][C:19]([O:21][CH2:22][CH:23]2[C:35]3[CH:34]=[CH:33][CH:32]=[CH:31][C:30]=3[C:29]3[C:24]2=[CH:25][CH:26]=[CH:27][CH:28]=3)=[O:20])=S)[CH:5]=1)[CH3:2]>O1CCOCC1.FC(F)(F)C([O-])=O.[Hg+2].FC(F)(F)C([O-])=O>[CH2:1]([O:3][C:4]1[C:9]([C:10](=[O:13])[NH:11][CH3:12])=[CH:8][N:7]2[C:16](=[N:18][C:19](=[O:20])[O:21][CH2:22][CH:23]3[C:35]4[CH:34]=[CH:33][CH:32]=[CH:31][C:30]=4[C:29]4[C:24]3=[CH:25][CH:26]=[CH:27][CH:28]=4)[NH:15][CH:14]=[C:6]2[CH:5]=1)[CH3:2]

参加物

4

反応物 1

HCID 57791308N-(4-Ethoxy-5-methylcarbamoylpyridin-2-ylmethyl)-N'-(fluoren-9-ylmethyloxycarbonyl)thiourea

生成物 1

HCID 1784658369H-Fluoren-9-ylmethyl (7-ethoxy-6-methylcarbamoyl-2H-imidazo[1,5-a]pyridin-3-ylidene)carbamate

試薬・触媒・溶媒 2

HCID 2723924Mercury bis(trifluoroacetate)触媒HCID 312751,4-Dioxane溶媒

実験手順

875 mg of N-(4-ethoxy-5-methylcarbamoyl pyridin-2-ylmethyl)-N′-(fluoren-9-ylmethyloxycarbonyl)thiourea (Example 19a, crude product) were dissolved in 25 ml of dioxane and treated at RT with 837 mg (1.96 mmol) of mercury(II) trifluoroacetate. After 10 minutes, the mixture was concentrated and the residue was taken up in DCM. The organic phase was washed three times with 4% strength LiCl solution and once with water, dried with MgSO4 and concentrated in a rotary evaporator. The crude product thus obtained (590 mg) was reacted further without further purification.

後処理

  1. concentrationthe mixture was concentrated
  2. washThe organic phase was washed three times with 4% strength LiCl solution
  3. dry with materialonce with water, dried with MgSO4
  4. concentrationconcentrated in a rotary evaporator

出典と根拠

ORDレコード
ord-8b381985904d458e8891b45a0d720ba1
出典データセット
uspto-grants-2011_01
特許番号
US07863269B2

関連ノート

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