Cesium carbonate → HCID 71655300, 화합물

HRID 270106

반응식

HRID 270106 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 71655300HCID 71655300, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-5da029fadcd84547a917c3e533b8f518
출처 데이터셋
uspto-grants-2008_11
특허 번호
US07449475B2

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