Lithium hydroxide, monohydrate → Di-tert-butyl 1-(1-acetylpiperidin-4-yl)hydrazine-1,2-dicarboxylate

HRID 44648노트

반응식

HRID 44648 반응식
[C:1]([N:4]1[CH2:9][CH2:8][CH:7]([N:10]([C:27]([O:29][C:30]([CH3:33])([CH3:32])[CH3:31])=[O:28])[N:11](C(=O)C2C=CC=CC=2)[C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13])[CH2:6][CH2:5]1)(=[O:3])[CH3:2].O.[OH-].[Li+]>O1CCCC1.O>[C:1]([N:4]1[CH2:5][CH2:6][CH:7]([N:10]([C:27]([O:29][C:30]([CH3:33])([CH3:32])[CH3:31])=[O:28])[NH:11][C:12]([O:14][C:15]([CH3:16])([CH3:17])[CH3:18])=[O:13])[CH2:8][CH2:9]1)(=[O:3])[CH3:2]

참가 물질

5

반응물 2

HCID 168937Lithium hydroxide, monohydrateHCID 68934227Di-tert-butyl 1-(1-acetylpiperidin-4-yl)-2-benzoylhydrazine-1,2-dicarboxylate

생성물 1

HCID 57444162Di-tert-butyl 1-(1-acetylpiperidin-4-yl)hydrazine-1,2-dicarboxylate수율 89.5%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

45 g (0.1 mol) of di-tert-butyl 1-(1-acetylpiperidin-4-yl)-2-benzoylhydrazine-1,2-dicarboxylate were dissolved in 1 L of tetrahydrofuran and a solution of 5.8 g (0.14 mol) of lithium hydroxide monohydrate in 1 L of water were added. The mixture was stirred at room temperature for 16 hours, the tetrahydrofuran removed in vacuo and the aqueous layer extracted several times with dichloromethane. The organic phase was dried over sodium sulfate and evaporated to dryness, giving 32 g (84% yield) of the title compound.

후처리

  1. customthe tetrahydrofuran removed in vacuo
  2. extractionthe aqueous layer extracted several times with dichloromethane
  3. dry with materialThe organic phase was dried over sodium sulfate
  4. customevaporated to dryness

출처 및 근거

ORD 기록
ord-98a349149d954d3498b5555fe29534a9
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08541429B2

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