Water → HCID 89835589, 화합물

HRID 2277091노트

반응식

HRID 2277091 반응식
[C:1]([O:4][C@H:5]([C:9]([CH3:12])([CH3:11])[CH3:10])[C:6](Cl)=[O:7])(=[O:3])[CH3:2].C(N(CC)CC)C.[CH3:20][O:21][C:22]([C@@H:24]1[CH2:29][N:28]([CH3:30])[CH2:27][CH2:26][NH:25]1)=[O:23].O>C(Cl)Cl>[CH3:20][O:21][C:22]([C@@H:24]1[CH2:29][N:28]([CH3:30])[CH2:27][CH2:26][N:25]1[C:6](=[O:7])[C@H:5]([O:4][C:1](=[O:3])[CH3:2])[C:9]([CH3:12])([CH3:11])[CH3:10])=[O:23]

참가 물질

6

반응물 4

HCID 962WaterHCID 8471TriethylamineHCID 44141012(S)-methyl-4-methylpiperazine-2-carboxylateHCID 89824898HCID 89824898, 화합물

생성물 1

HCID 89835589HCID 89835589, 화합물수율 40.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a stirred solution of (2R)-1-chloro-3,3-dimethyl-1-oxobutan-2-yl acetate (0.247 g, 1.41 mmol) in CH2Cl2 (10 mL) was added triethylamine (0.39 mL, 2.83 mmol) and a solution of (S)-methyl-4-methylpiperazine-2-carboxylate (0.150 g, 0.943 mmol) in CH2Cl2 (3 mL) dropwise. The reaction mixture was stirred at room temperature for 30 minutes. Water (10 mL) was then added to quench the reaction and the reaction mixture was extracted with CH2Cl2 (2×25 mL). The combined organic layers were separated, washed with water (2×50 mL) dried over Na2SO4 and concentrated under reduced pressure to afford the title compound (0.12 g) as a white solid.

후처리

  1. customto quench
  2. customthe reaction
  3. extractionthe reaction mixture was extracted with CH2Cl2 (2×25 mL)
  4. customThe combined organic layers were separated
  5. washwashed with water (2×50 mL)
  6. dry with materialdried over Na2SO4
  7. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-f052adda9a9d43afa71a9b611c74f162
출처 데이터셋
uspto-grants-2015_09
특허 번호
US09133147B2

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