Cesium carbonate → HCID 54500758, 화합물

HRID 1421748노트

반응식

HRID 1421748 반응식
[CH3:1][O:2][C:3](=[O:13])[C:4]1[CH:9]=[CH:8][C:7]([C:10]#[N:11])=[C:6]([OH:12])[CH:5]=1.[C:14]1([CH2:20][CH2:21][CH2:22][CH2:23]Cl)[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1.C([O-])([O-])=O.[Cs+].[Cs+]>CN(C=O)C>[CH3:1][O:2][C:3](=[O:13])[C:4]1[CH:9]=[CH:8][C:7]([C:10]#[N:11])=[C:6]([O:12][CH2:23][CH2:22][CH2:21][CH2:20][C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[CH:5]=1

참가 물질

5

반응물 3

HCID 10796Cesium carbonateHCID 78543(4-Chlorobutyl)benzeneHCID 16641129Methyl 4-cyano-3-hydroxybenzoate

생성물 1

HCID 54500758HCID 54500758, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

4-Cyano-3-hydroxybenzoic acid methyl ester, Example 34 Step 3 (300 mg, 1.7 mmol) was dissolved in DMF (85 ml) and treated with phenylbutylchloride (287 mg, 1.7 mmol). Cs2CO3 (610 mg, 1.87 mmol) was then added and the reaction mixture stirred at room temp. for 18 hours. The mixture was filtered and washed with DMF (3×10 mL). The solvent was removed in vacuo and the residue was purified by flash chromatography (10% EtOAc/Hexane) to yield desired product.

후처리

  1. filtrationThe mixture was filtered
  2. washwashed with DMF (3×10 mL)
  3. customThe solvent was removed in vacuo
  4. customthe residue was purified by flash chromatography (10% EtOAc/Hexane)

출처 및 근거

ORD 기록
ord-bea1ed27dbf54b2eb3f073c28bd79230
출처 데이터셋
uspto-grants-2000_06
특허 번호
US06077853

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