Sodium Chloride → (S)-4-Benzyl 1-tert-butyl 2-ethyl piperazine-1,2,4-tricarboxylate

HRID 1006348노트

반응식

HRID 1006348 반응식
C(O)(=O)[C@H]([C@@H](C(O)=O)O)O.[C:11]([O:15][C:16]([N:18]1[CH2:23][CH2:22][NH:21][CH2:20][C@H:19]1[C:24]([O:26][CH2:27][CH3:28])=[O:25])=[O:17])([CH3:14])([CH3:13])[CH3:12].C(=O)(O)[O-].[Na+].Cl[C:35]([O:37][CH2:38][C:39]1[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=1)=[O:36].[Cl-].[Na+]>O1CCCC1.O.C(OCC)(=O)C>[C:11]([O:15][C:16]([N:18]1[CH2:23][CH2:22][N:21]([C:35]([O:37][CH2:38][C:39]2[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=2)=[O:36])[CH2:20][C@H:19]1[C:24]([O:26][CH2:27][CH3:28])=[O:25])=[O:17])([CH3:14])([CH3:13])[CH3:12]

참가 물질

8

반응물 4

HCID 5234Sodium ChlorideHCID 10387Benzyl chloroformateHCID 516892Sodium BicarbonateHCID 86589649(2S)-2-ethoxycarbonylpiperazine-1-carboxylic acid 1-tert-butyl ester D-tartarate

생성물 1

HCID 59016652(S)-4-Benzyl 1-tert-butyl 2-ethyl piperazine-1,2,4-tricarboxylate

시약·촉매·용매 3

HCID 962Water용매HCID 8028Tetrahydrofuran용매HCID 8857Ethyl Acetate용매

실험 절차

To a solution of (2S)-2-ethoxycarbonylpiperazine-1-carboxylic acid 1-tert-butyl ester D-tartarate (9.56 g) in tetrahydrofuran (90 ml) and water (90 ml) was added sodium bicarbonate (7.87 g) under ice-cooling. Benzyl chloroformate (4.01 ml) was added dropwise to the solution over 2 minutes at the same temperature, and stirred at room temperature for 15 minutes. Ethyl acetate (60 ml) and sodium chloride (5 g) was added to the mixture. The organic layer was washed with brine, dried over magnesium sulfate, and evaporated under reduced pressure to give (2S)-2-ethoxycarbonylpiperazine-1,4-dicarboxylic acid 4-benzyl ester 1-tert-butyl ester (10.4 g) as a colorless oil.

후처리

  1. temperaturecooling
  2. washThe organic layer was washed with brine
  3. dry with materialdried over magnesium sulfate
  4. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-b7d0afa322964a468c2aae6915b222d7
출처 데이터셋
uspto-grants-2004_09
특허 번호
US06787543B2

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