Triethylamine → HCID 178481869、化合物

HRID 1247779

反応式

HRID 1247779 の反応式
[C:1]([O:5][C:6]([NH:8][C:9]([NH:18][C:19]([O:21][C:22]([CH3:25])([CH3:24])[CH3:23])=[O:20])=[N:10]S(C(F)(F)F)(=O)=O)=[O:7])([CH3:4])([CH3:3])[CH3:2].S(=O)(=O)(O)O.N[C:32]1[CH:33]=[N:34][N:35]([CH3:38])[C:36]=1[NH2:37].C(N(CC)CC)C.C(OCC)(=O)C>ClCCl.O>[NH2:37][C:36]1[N:35]([CH3:38])[N:34]=[CH:33][C:32]=1[NH:10][C:9]([NH:18][C:19]([O:21][C:22]([CH3:25])([CH3:24])[CH3:23])=[O:20])=[N:8][C:6]([O:5][C:1]([CH3:4])([CH3:3])[CH3:2])=[O:7]

参加物

7

反応物 4

HCID 8471TriethylamineHCID 8857Ethyl AcetateHCID 36945701,3-Di-Boc-2-(trifluoromethylsulfonyl)guanidineHCID 219045711H-Pyrazole, 4,5-diamine-1-methyl-, sulfate (1:1)

生成物 1

HCID 178481869HCID 178481869、化合物収率 68.9%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

To a solution of 1,3-bis(tert-butoxycarbonyl)-2-(trifluoromethylsulfonyl)guanidine (22.3 g) in dichloromethane (100 ml) were added 4,5-diamino-1-methylpyrazole sulfuric acid salt (10 g) and triethylamine (33.2 ml) at 4° C., and the mixture was stirred at room temperature overnight. The reaction mixture was poured into a mixture of ethyl acetate and water. The aqueous layer was separated, and the organic layer was washed with brine, dried over anhydrous magnesium sulfate and filtered. The filtrate was concentrated in vacuo. The concentrate was poured into acetonitrile, and the resulting precipitate was collected by filtration and dried in vacuo to give 5-amino-4-[2′,3′-bis(tert-butoxycarbonyl)guanidino]-1-methylpyrazole (11.62 g).

後処理

  1. customThe aqueous layer was separated
  2. washthe organic layer was washed with brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. concentrationThe filtrate was concentrated in vacuo
  6. additionThe concentrate was poured into acetonitrile
  7. filtrationthe resulting precipitate was collected by filtration
  8. customdried in vacuo

出典と根拠

ORDレコード
ord-2712a3eda6524cefae95afae20296eb2
出典データセット
uspto-grants-2006_10
特許番号
US07129232B2

関連ノート

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