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Dichloromethane → 4-(4-But-2-ynyloxy-benzenesulfonylmethyl)-piperidine-1,4-dicarboxylic acid ethyl ester methyl ester

HRID 353559
ノート
印刷プレビュー

反応式

HRID 353559 の反応式
C([O:3][C:4]([C:6]1([CH2:12][S:13]([C:16]2[CH:21]=[CH:20][C:19]([O:22][CH2:23][C:24]#[C:25][CH3:26])=[CH:18][CH:17]=2)(=[O:15])=[O:14])[CH2:11][CH2:10][NH:9][CH2:8][CH2:7]1)=[O:5])C.[CH3:27]/[C:28](/[O:34][Si](C)(C)C)=N\[Si](C)(C)C.[CH3:39][O:40]C(Cl)=O.[CH2:44](Cl)Cl>>[CH3:44][O:3][C:4]([C:6]1([CH2:12][S:13]([C:16]2[CH:21]=[CH:20][C:19]([O:22][CH2:23][C:24]#[C:25][CH3:26])=[CH:18][CH:17]=2)(=[O:14])=[O:15])[CH2:11][CH2:10][N:9]([C:39]([O:34][CH2:28][CH3:27])=[O:40])[CH2:8][CH2:7]1)=[O:5]
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

5

反応物 4

HCID 6344Dichloromethane3 回HCID 6586Methyl chloroformateHCID 6913588N,O-bis(trimethylsilyl)acetamideHCID 22626999HCID 22626999、化合物

生成物 1

HCID 538996104-(4-But-2-ynyloxy-benzenesulfonylmethyl)-piperidine-1,4-dicarboxylic acid ethyl ester methyl ester収率 85%

反応条件

温度
0 °C

実験手順

To a solution of 4-[[[4-(2-Butynyloxy)phenyl]sulfonyl]methyl]-4-piperidinecarboxylic acid ethyl ester (0.354 g, 0.85 mmol) in 1.0 mL of CH2Cl2 under N2 atmosphere was added dropwise a solution of N,O-bis(trimethylsilyl)acetamide (0.462 ml, 1.87 mmol) in 0.5 mL of CH2Cl2 and stirred for 1 h The reaction was cooled to 0° C. and added dropwise a solution of 0.079 mL (1.02 mmol) of methylchloroformate in 0.5 mL of CH2Cl2. The reaction was allowed to stir at room temperature for 1 hand cooled to 0° C., quenched with pH 7 buffer solution and extracted with EtOAc. The organics was washed with H2O, brine, dried over MgSO4, filtered, and concentrated in vacuo. The residue was chromatographed on silica gel eluting with EtOAc:hexanes (1:2) to provide 0.315 g (85%) of the desired product as a colorless oil. Electrospray Mass Spec: 438.3 (M+H)+.

後処理

  1. stirringto stir at room temperature for 1 hand
  2. temperaturecooled to 0° C.
  3. customquenched with pH 7 buffer solution
  4. extractionextracted with EtOAc
  5. washThe organics was washed with H2O, brine
  6. dry with materialdried over MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo
  9. customThe residue was chromatographed on silica gel eluting with EtOAc:hexanes (1:2)

出典と根拠

ORDレコード
ord-a6523a690d084aaea0ad23a8d01b5050
出典データセット
uspto-grants-2004_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06753337B2

反応ノート

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