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Citric Acid → 1-(tert-Butoxycarbonyl)-4-(4-chlorobenzoylmethanesulfonyl)piperazine

HRID 278577
ノート
印刷プレビュー

反応式

HRID 278577 の反応式
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][N:11]([S:14]([CH3:17])(=[O:16])=[O:15])[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].C([Li])CCC.[Cl:23][C:24]1[CH:33]=[CH:32][C:27]([C:28](OC)=[O:29])=[CH:26][CH:25]=1.C(O)(=O)CC(CC(O)=O)(C(O)=O)O>O1CCCC1.CCCCCC.O>[C:1]([O:5][C:6]([N:8]1[CH2:9][CH2:10][N:11]([S:14]([CH2:17][C:28](=[O:29])[C:27]2[CH:32]=[CH:33][C:24]([Cl:23])=[CH:25][CH:26]=2)(=[O:15])=[O:16])[CH2:12][CH2:13]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 311Citric AcidHCID 14307Methyl 4-chlorobenzoateHCID 4496004Tert-butyl 4-(methylsulfonyl)piperazine-1-carboxylateHCID 178418339Butyllithium

生成物 1

HCID 226282031-(tert-Butoxycarbonyl)-4-(4-chlorobenzoylmethanesulfonyl)piperazine収率 39.3%

試薬・触媒・溶媒 3

HCID 962
Water
溶媒
HCID 8028Tetrahydrofuran溶媒2 回
HCID 8058Hexane溶媒

反応条件

温度
-78 °C

実験手順

To a solution of 1-(tert-butoxycarbonyl)-4-methanesulfonylpiperazine (1.32 g) in tetrahydrofurane (10 ml) was added dropwise at 0° C. 1.6 M n-butyllithium in hexane (6.25 ml), and the mixture was stirred at room temperature for 30 minutes. The reaction solution was cooled to −78° C., and to the mixture was added a solution of methyl 4-chlorobenzoate (853 mg) in tetrahydrofurane (5 ml). The mixture was stirred for 3 hours at the same temperature and raised to 0° C. To the reaction solution was added water (10 ml), and the mixture was made acidic with citric acid aqueous solution and extracted with ether. The organic layer was washed with brine, dried, concentrated, and purified with silica gel column chromatography (hexane/ethyl acetate=2/1) to give a colorless solid of the title compound (790 mg).

後処理

  1. temperatureraised to 0° C
  2. extractionextracted with ether
  3. washThe organic layer was washed with brine
  4. customdried
  5. concentrationconcentrated
  6. custompurified with silica gel column chromatography (hexane/ethyl acetate=2/1)

出典と根拠

ORDレコード
ord-b2cc35848a47496aa0f74711eea76541
出典データセット
uspto-grants-2002_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06359134B1

反応ノート

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