Hydrochloric Acid → 4-[4-(1-benzofuran-5-yl)phenyl]-5-[(3S)-3-pyrrolidinylmethyl]-2,4-dihydro-3H-1,2,4-triazol-3-one hydrochloride

HRID 525167ノート

反応式

HRID 525167 の反応式
[O:1]1[C:5]2[CH:6]=[CH:7][C:8]([C:10]3[CH:15]=[CH:14][C:13]([N:16]4[C:20](=[O:21])[NH:19][N:18]=[C:17]4[CH2:22][C@@H:23]4[CH2:27][CH2:26][N:25](C(OC(C)(C)C)=O)[CH2:24]4)=[CH:12][CH:11]=3)=[CH:9][C:4]=2[CH:3]=[CH:2]1.O1CCOCC1.[ClH:41]>>[ClH:41].[O:1]1[C:5]2[CH:6]=[CH:7][C:8]([C:10]3[CH:15]=[CH:14][C:13]([N:16]4[C:17]([CH2:22][C@@H:23]5[CH2:27][CH2:26][NH:25][CH2:24]5)=[N:18][NH:19][C:20]4=[O:21])=[CH:12][CH:11]=3)=[CH:9][C:4]=2[CH:3]=[CH:2]1

参加物

4

反応物 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 67376548tert-butyl (3S)-3-({4-[4-(1-benzofuran-5-yl)phenyl]-5-oxo-4,5-dihydro-1H-1,2,4-triazol-3-yl}methyl)pyrrolidine-1-carboxylate

生成物 1

HCID 673758814-[4-(1-benzofuran-5-yl)phenyl]-5-[(3S)-3-pyrrolidinylmethyl]-2,4-dihydro-3H-1,2,4-triazol-3-one hydrochloride収率 96%

実験手順

In a round bottom flask under nitrogen, a yellow mixture of tert-butyl (3S)-3-({4-[4-(1-benzofuran-5-yl)phenyl]-5-oxo-4,5-dihydro-1H-1,2,4-triazol-3-yl}methyl)pyrrolidine-1-carboxylate (2.58 g, 5.60 mmol) in 4M HCl in dioxane (1.40 mL, 5.60 mmol) was stirred at room temperature for 30 min. The reaction mixture was concentrated in vacuo. Ethanol (300 mL) was added to the flask and the solvent was removed by concentration in vacuo to give the title compound as a cream coloured solid (2.14 g, 96%). MS(ES)+ m/e 361.1 [M+H]+.

後処理

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. additionEthanol (300 mL) was added to the flask
  3. customthe solvent was removed by concentration in vacuo

出典と根拠

ORDレコード
ord-286bb7e22e26454cb1e8246cbf6c7599
出典データセット
uspto-grants-2016_05
特許番号
US09340529B2

反応ノート

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