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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
ノート
印刷プレビュー

反応式

HRID 1773787 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 312751,4-Dioxane溶媒

実験手順

[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.

後処理

  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

出典と根拠

ORDレコード
ord-4aa2d27bf6894288b2b96ee75056f6a5
出典データセット
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09255103B2

反応ノート

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