Water → HCID 89835589、化合物

HRID 2277091ノート

反応式

HRID 2277091 の反応式
[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]

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 44141012(S)-methyl-4-methylpiperazine-2-carboxylateHCID 89824898HCID 89824898、化合物

生成物 1

HCID 89835589HCID 89835589、化合物収率 40.5%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f052adda9a9d43afa71a9b611c74f162
出典データセット
uspto-grants-2015_09
特許番号
US09133147B2

反応ノート

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