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Hydrochloric Acid → 1-ethyl-3-[2-oxo-2-(1-pyrrolidinyl)ethyl]-1H-pyrazol-5-amine

HRID 1472544
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HRID 1472544 반응식
[CH2:1]([N:3]1[C:7]([NH:8]C(=O)C(F)(F)F)=[CH:6][C:5]([CH2:15][C:16](=[O:22])[N:17]2[CH2:21][CH2:20][CH2:19][CH2:18]2)=[N:4]1)[CH3:2].Cl>CO>[CH2:1]([N:3]1[C:7]([NH2:8])=[CH:6][C:5]([CH2:15][C:16](=[O:22])[N:17]2[CH2:18][CH2:19][CH2:20][CH2:21]2)=[N:4]1)[CH3:2]
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4

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HCID 313Hydrochloric AcidHCID 59314454N-{1-Ethyl-3-[2-oxo-2(1-pyrrolidinyl)ethyl]-1H-pyrazol-5-yl}-2,2,2-trifluoroacetamide

생성물 1

HCID 575169011-ethyl-3-[2-oxo-2-(1-pyrrolidinyl)ethyl]-1H-pyrazol-5-amine

시약·촉매·용매 1

HCID 887Methanol용매

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온도
50 °C

실험 절차

To a solution of N-{1-ethyl-3-[2-oxo-2-(1-pyrrolidinyl)ethyl]-1H-pyrazol-5-yl}-2,2,2-trifluoroacetamide (120 mg, 0.377 mmol) in methanol (1.5 mL) was added 2M HCl (1 mL, 0.377 mmol), and the reaction mixture was stirred at 50° C. for 2 h and concentrated. The residue was neutralized using saturated NaHCO3 solution and concentrated. The residue was dried under high vacuum to give 79 mg and used for next reaction without further purification. MS: (M+H)+=222.8. 1H NMR (400 MHz, DMSO-d6) ppm 1.18 (t, J=7.2 Hz, 3H), 1.70-1.85 (m, 4 H), 3.24 (t, J=6.8 Hz, 2H), 3.31 (s, 2 H), 3.43 (t, J=6.8 Hz, 2H), 3.78 (q, J=7.2 Hz, 2H), 5.11 (s, 1H).

후처리

  1. concentrationconcentrated
  2. concentrationconcentrated
  3. customThe residue was dried under high vacuum
  4. customto give 79 mg
  5. customused for next reaction without further purification

출처 및 근거

ORD 기록
ord-bd64c682bc184a638d533295ea5cf7e5
출처 데이터셋
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09012479B2

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