Cesium carbonate → HCID 86612855, 화합물

HRID 1782032

반응식

HRID 1782032 반응식
[OH:1][C:2]1[CH:7]=[C:6]([O:8][CH3:9])[CH:5]=[CH:4][C:3]=1[CH2:10][C:11]([NH:13][CH3:14])=[O:12].[N+](C1C=C(S(O[CH2:28][C@@H:29]2[CH2:31][O:30]2)(=O)=O)C=CC=1)([O-])=O.C([O-])([O-])=O.[Cs+].[Cs+]>CN(C=O)C>[CH3:9][O:8][C:6]1[CH:5]=[CH:4][C:3]([CH2:10][C:11]([NH:13][CH3:14])=[O:12])=[C:2]([O:1][CH2:28][C@@H:29]2[CH2:31][O:30]2)[CH:7]=1

참가 물질

5

반응물 3

HCID 10796Cesium carbonateHCID 146490Benzenesulfonic acid, 3-nitro-, (2S)-2-oxiranylmethyl esterHCID 690173522-(2-hydroxy-4-methoxyphenyl)-N-methylacetamide

생성물 1

HCID 86612855HCID 86612855, 화합물수율 94.3%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A mixture of 2-(2-hydroxy-4-methoxyphenyl)-N-methylacetamide (15 mg, 0.076 mmol), (2S)-oxiran-2-ylmethyl 3-nitrobenzenesulfonate (20 mg, 0.076 mmol) and Cs2CO3 (30 mg, 0.091 mmol) in DMF (1.5 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 (0-100% ethyl acetate in petroleum spirit) to give the subtitled compound (18 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 (0-100% ethyl acetate in petroleum spirit)

출처 및 근거

ORD 기록
ord-bdf2fce010bd419281858860233fc2c2
출처 데이터셋
uspto-grants-2009_03
특허 번호
US07498338B2

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