Sodium Hydroxide → 1-(3-Methyl-1,2,4-thiadiazol-5-yl)piperidin-4-amine

HRID 451461ノート

反応式

HRID 451461 の反応式
Cl.Cl.[CH3:3][C:4]1[N:8]=[C:7]([N:9]2[CH2:14][CH2:13][CH:12]([NH2:15])[CH2:11][CH2:10]2)[S:6][N:5]=1.[OH-].[Na+]>>[CH3:3][C:4]1[N:8]=[C:7]([N:9]2[CH2:10][CH2:11][CH:12]([NH2:15])[CH2:13][CH2:14]2)[S:6][N:5]=1

参加物

3

反応物 2

HCID 14798Sodium HydroxideHCID 673442811-(3-Methyl-1,2,4-thiadiazol-5-yl)piperidin-4-amine dihydrochloride

生成物 1

HCID 583978761-(3-Methyl-1,2,4-thiadiazol-5-yl)piperidin-4-amine

実験手順

1-(3-Methyl-1,2,4-thiadiazol-5-yl)piperidin-4-amine dihydrochloride (see example 36b, 2.3 g, 8.48 mmol) was neutralized with 2 N NaOH solution, The water layer was extracted three times with CH2Cl2 and three times with ethyl acetate, the combined organic phases were dried over Na2SO4, filtered and the solvents were evaporated. The crude product was purified by flash chromatography with CH2Cl2 and MeOH over a 50 g Si—NH2 column. The title compound was isolated as a light yellow oil (1.2 g, 71%).

後処理

  1. extractionThe water layer was extracted three times with CH2Cl2 and three times with ethyl acetate
  2. dry with materialthe combined organic phases were dried over Na2SO4
  3. filtrationfiltered
  4. customthe solvents were evaporated
  5. customThe crude product was purified by flash chromatography with CH2Cl2 and MeOH over a 50 g Si—NH2 column

出典と根拠

ORDレコード
ord-9734e21d11de4deeb00f28af8d2fbf88
出典データセット
uspto-grants-2013_07
特許番号
US08486967B2

反応ノート

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