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Acetic Acid → 4-(2-Carboxy-2-ethoxy-ethyl)-benzoic acid 4-methanesulfonyloxy-benzyl ester

HRID 1628190
ノート
印刷プレビュー

反応式

HRID 1628190 の反応式
[CH3:1][S:2]([O:5][C:6]1[CH:34]=[CH:33][C:9]([CH2:10][O:11][C:12](=[O:32])[C:13]2[CH:18]=[CH:17][C:16]([CH2:19][CH:20]([O:29][CH2:30][CH3:31])[C:21]([O:23]CC(Cl)(Cl)Cl)=[O:22])=[CH:15][CH:14]=2)=[CH:8][CH:7]=1)(=[O:4])=[O:3].C(O)(=O)C>C(Cl)Cl.[Zn]>[CH3:1][S:2]([O:5][C:6]1[CH:7]=[CH:8][C:9]([CH2:10][O:11][C:12](=[O:32])[C:13]2[CH:18]=[CH:17][C:16]([CH2:19][CH:20]([C:21]([OH:23])=[O:22])[O:29][CH2:30][CH3:31])=[CH:15][CH:14]=2)=[CH:33][CH:34]=1)(=[O:4])=[O:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 176Acetic AcidHCID 866503074-[2-Ethoxy-2-(2,2,2-trichloro-ethoxycarbonyl)-ethyl]-benzoic acid 4-methane sulfonyloxy-benzyl ester

生成物 1

HCID 866503144-(2-Carboxy-2-ethoxy-ethyl)-benzoic acid 4-methanesulfonyloxy-benzyl ester

試薬・触媒・溶媒 2

HCID 23994Zinc触媒HCID 6344Dichloromethane溶媒

実験手順

To a solution of 4-[2-ethoxy-2-(2,2,2-trichloro-ethoxycarbonyl)-ethyl]-benzoic acid 4-methane sulfonyloxy-benzyl ester (0.02 g, 0.036 mmol) in dry DCM (2 mL) was first added zinc dust (0.047 g, 0.722 mmol), then acetic acid (1.08 mL, 18.06 mmol) at 0° C. The resulting inhomogenous mixture was stirred for 17 h without removing the ice bath. The zinc was filtered off and washed with DCM and MeOH and the remaining filtrates were combined and evaporated under reduced pressure. The crude product was purified by column chromatography using DCM/MeOH (92:8) as the eluent. The title compound was obtained as an oil (0.005 g, 36%). 1H NMR (400 MHz, CDCl3): δ 7.91-7.93 (d, 2H), 7.42-7.44 (d, 2H, 7.19-7.24 (m, 4H), 5.27 (s, 2H), 4.03 (m, 1H), 3.52 (m, 1H), 3.37 (m, 1H), 2.99-3.14 (m, 2H), 3.08 (s, 3H), 2.63 (t, 3H). Mass Spectrum: M−H+ 421.23.

後処理

  1. customat 0° C
  2. customwithout removing the ice bath
  3. filtrationThe zinc was filtered off
  4. washwashed with DCM and MeOH
  5. customevaporated under reduced pressure
  6. customThe crude product was purified by column chromatography

出典と根拠

ORDレコード
ord-1a8a4b4a87c942f2bf74aab0dc6fcc16
出典データセット
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08785681B2

反応ノート

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