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

HRID 451461노트

반응식

HRID 451461 반응식
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

참가 물질

3

반응물 2

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

생성물 1

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

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-9734e21d11de4deeb00f28af8d2fbf88
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08486967B2

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