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[2-(5-Acetyl-3-phenoxymethyl-pyrazol-1-yl)-ethyl]-carbamic acid tert-butyl ester → 4-Methyl-2-phenoxymethyl-6,7-dihydro-pyrazolo[1,5-a]pyrazine

HRID 1773787
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반응식

HRID 1773787 반응식
C(OC(=O)[NH:7][CH2:8][CH2:9][N:10]1[C:14]([C:15](=O)[CH3:16])=[CH:13][C:12]([CH2:18][O:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)=[N:11]1)(C)(C)C>Cl.O1CCOCC1>[CH3:16][C:15]1[C:14]2[N:10]([N:11]=[C:12]([CH2:18][O:19][C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=3)[CH:13]=2)[CH2:9][CH2:8][N:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 67958451[2-(5-Acetyl-3-phenoxymethyl-pyrazol-1-yl)-ethyl]-carbamic acid tert-butyl ester

생성물 1

HCID 679598694-Methyl-2-phenoxymethyl-6,7-dihydro-pyrazolo[1,5-a]pyrazine수율 99.9%

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 312751,4-Dioxane용매

실험 절차

[2-(5-Acetyl-3-phenoxymethyl-pyrazol-1-yl)-ethyl]-carbamic acid tert-butyl ester (0.2 g, 0.56 mmol) was dissolved in a 4M solution of HCl in 1,4-dioxane (2.12 mL) under nitrogen. The mixture was stirred at room temperature for 30 minutes and then the solvents evaporated in vacuo. The residue was basified with a saturated solution of Na2CO3 and extracted with DCM. The organic layer was separated, dried (Na2SO4), filtered and the solvents evaporated in vacuo to yield 4-methyl-2-phenoxymethyl-6,7-dihydro-pyrazolo[1,5-a]pyrazine (135 mg, 99% yield) as a brown solid that was used without further purification.

후처리

  1. customthe solvents evaporated in vacuo
  2. extractionextracted with DCM
  3. customThe organic layer was separated
  4. dry with materialdried (Na2SO4)
  5. filtrationfiltered
  6. customthe solvents evaporated in vacuo

출처 및 근거

ORD 기록
ord-4aa2d27bf6894288b2b96ee75056f6a5
출처 데이터셋
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09255103B2

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