Cesium carbonate → HCID 71655300、化合物

HRID 270106

反応式

HRID 270106 の反応式
[N+](C1C=C(S(O[CH2:14][C@@H:15]2[CH2:17][O:16]2)(=O)=O)C=CC=1)([O-])=O.[OH:18][C:19]1[CH:28]=[C:27]([CH3:29])[CH:26]=[CH:25][C:20]=1[C:21]([O:23][CH3:24])=[O:22].C([O-])([O-])=O.[Cs+].[Cs+]>CN(C=O)C>[CH3:29][C:27]1[CH:26]=[CH:25][C:20]([C:21]([O:23][CH3:24])=[O:22])=[C:19]([O:18][CH2:14][C@@H:15]2[CH2:17][O:16]2)[CH:28]=1

参加物

5

反応物 3

HCID 10796Cesium carbonateHCID 78400Benzoic acid, 2-hydroxy-4-methyl-, methyl esterHCID 146490Benzenesulfonic acid, 3-nitro-, (2S)-2-oxiranylmethyl ester

生成物 1

HCID 71655300HCID 71655300、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of (2S)-oxiran-2-ylmethyl 3-nitrobenzenesulfonate (777.7 mg, 3.0 mmol), methyl 2-hydroxy-4-methylbenzoate ((498.5 mg, 3.0 mmol) and Cs2CO3 (1.17 g, 3.6 mmol) in DMF (10 mL) was stirred at room temperature overnight. The reaction mixture was partitioned between ethyl acetate and H2O. The organic layer was dried over Na2SO4, filtered and concentrated. The residue was purified by silica gel flash chromatography (0-20% ethyl acetate in petroleum spirit) to give the subtitled compound (500 mg).

後処理

  1. customThe reaction mixture was partitioned between ethyl acetate and H2O
  2. dry with materialThe organic layer was dried over Na2SO4
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customThe residue was purified by silica gel flash chromatography (0-20% ethyl acetate in petroleum spirit)

出典と根拠

ORDレコード
ord-5da029fadcd84547a917c3e533b8f518
出典データセット
uspto-grants-2008_11
特許番号
US07449475B2

関連ノート

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