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 2405349노트

반응식

HRID 2405349 반응식
[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

참가 물질

4

반응물 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

생성물 1

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

실험 절차

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]+.

후처리

  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

출처 및 근거

ORD 기록
ord-8e9dc5d168664421b59ce55844624406
출처 데이터셋
uspto-grants-2014_08
특허 번호
US08802864B2

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