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Trimethylsilyl triflate → HCID 66992487、化合物

HRID 556727
ノート
印刷プレビュー

反応式

HRID 556727 の反応式
[C:1]([O:9][CH:10]1[CH2:15][CH2:14][CH2:13][CH2:12][CH:11]1[OH:16])(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.FC(F)(F)S(O[Si](C)(C)C)(=O)=O.ClC(Cl)(Cl)C(=N)O[CH2:33][CH2:34][C:35]1[CH:40]=[CH:39][C:38]([O:41][CH3:42])=[C:37]([O:43][CH3:44])[CH:36]=1>C(Cl)Cl>[C:1]([O:9][C@@H:10]1[CH2:15][CH2:14][CH2:13][CH2:12][C@@H:11]1[O:16][CH2:33][CH2:34][C:35]1[CH:40]=[CH:39][C:38]([O:41][CH3:42])=[C:37]([O:43][CH3:44])[CH:36]=1)(=[O:8])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
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 3

HCID 65367Trimethylsilyl triflateHCID 4687839HCID 4687839、化合物HCID 16743807Ethanimidic acid, 2,2,2-trichloro-, 2-(3,4-dimethoxyphenyl)ethyl ester

生成物 1

HCID 66992487HCID 66992487、化合物収率 67.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
0 °C

実験手順

A 250 mL round bottom flask equipped with an argon inlet and magnetic stir bar was charged with 2-hydroxycyclohexyl benzoate (7.39 g, 33.6 mmol) in anhydrous CH2Cl2 (50 mL). The solution was cooled to 0° C. prior to the successive addition of trimethylsilyl trifluoromethanesulfonate (3.0 mL, 1.9.4 mmol) and 3,4-dimethoxyphenethyl 2,2,2-trichloroacetimidate (16.5 g, 50.4 mmol) dissolved in anhydrous CH2Cl2 (30 mL). The reaction mixture was stirred at r.t. for 3 days. The reaction was then quenched by the addition of H2O (100 mL). The aqueous layer was extracted with CH2Cl2 (3×100 mL). The combined organic extracts were washed successively with brine (2×100 mL) and distilled water (100 mL), dried over anhydrous MgSO4, and concentrated under vacuum. The crude material was purified by flash column chromatography (EtOAc-hexanes, 1:7, v/v,) to afford a yellow oil (8.69 g, 67%). Rf 0.77 (EtOAc-hexanes, 1:2, v/v,); 1H-NMR (300 MHz, CDCl3) δ 1.36 (m, 2H), 1.62 (m, 4H), 1.85-2.03 (m, 2H), 2.75 (t, 2H), 3.53 (m, 1H), 3.62 (m, 1H), 3.72 (m, 2H), 3.79 (s, 6H, OCH3), 6.76 (m, 3H, Ar), 7.38 (m, 2H, Ar), 7.53 (m, 1H, Ar), 8.00 (m, 2H, Ar).

後処理

  1. customA 250 mL round bottom flask equipped with an argon inlet and magnetic stir bar
  2. customThe reaction was then quenched by the addition of H2O (100 mL)
  3. extractionThe aqueous layer was extracted with CH2Cl2 (3×100 mL)
  4. washThe combined organic extracts were washed successively with brine (2×100 mL)
  5. distillationdistilled water (100 mL)
  6. dry with materialdried over anhydrous MgSO4
  7. concentrationconcentrated under vacuum
  8. customThe crude material was purified by flash column chromatography (EtOAc-hexanes, 1:7, v/v,)

出典と根拠

ORDレコード
ord-ea834d42a68446e19edfdf3f854a1b83
出典データセット
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08058304B2

反応ノート

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