Acetic Acid → 3-Tert-butyl-1-((tetrahydro-2h-pyran-2-yl)methyl)-1h-pyrazol-5-amine

HRID 452974

反応式

[C:1]([C:5]1[CH:9]=[C:8](/[N:10]=C/N(C)C)[N:7]([CH2:15][CH:16]2[CH2:21][CH2:20][CH2:19][CH2:18][O:17]2)[N:6]=1)([CH3:4])([CH3:3])[CH3:2].NN.C(O)(=O)C>O1CCOCC1>[C:1]([C:5]1[CH:9]=[C:8]([NH2:10])[N:7]([CH2:15][CH:16]2[CH2:21][CH2:20][CH2:19][CH2:18][O:17]2)[N:6]=1)([CH3:4])([CH3:2])[CH3:3]

参加物

反応条件

温度: 85 °C

実験手順

To a solution of Example 63B (0.9 g, 3.1 mmol) in dioxane (10 mL) were added hydrazine (0.12 mL, 3.7 mmol, Aldrich) and acetic acid (0.35 mL, 6.2 mmol). After stirring at 85° C. for 16 hours, the reaction mixture was cooled and quenched with saturated NaHCO3 (10 mL). The aqueous layer was extracted with ethyl acetate (3×20 mL). The combined organic extracts were dried over anhydrous Na2SO4, filtered and concentrated under reduced pressure to provide the title compound. MS (APCI+) m/z 238 (M+H)+.

後処理

temperaturethe reaction mixture was cooled
customquenched with saturated NaHCO3 (10 mL)
extractionThe aqueous layer was extracted with ethyl acetate (3×20 mL)
dry with materialThe combined organic extracts were dried over anhydrous Na2SO4
filtrationfiltered
concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード: ord-9f1e66612f644f2380608be7ebeefcdd
出典データセット: uspto-grants-2013_07
DOI: 10.6084/m9.figshare.5104873.v1
特許番号: US08492371B2

反応式

参加物

反応物 3

生成物 1

試薬・触媒・溶媒 1

反応条件

実験手順

後処理

出典と根拠

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