Methyl iodide → Methyl 2-(1,3-dioxaindan-5-yl)acetate

HRID 274926

반응식

HRID 274926 반응식
[CH2:1]1[O:9][C:8]2[CH:7]=[CH:6][C:5]([CH2:10][C:11]([OH:13])=[O:12])=[CH:4][C:3]=2[O:2]1.[C:14](=O)([O-])[O-].[Cs+].[Cs+].CI>CN(C=O)C>[CH2:1]1[O:9][C:8]2[CH:7]=[CH:6][C:5]([CH2:10][C:11]([O:13][CH3:14])=[O:12])=[CH:4][C:3]=2[O:2]1

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 10796Cesium carbonateHCID 76115Benzo-1,3-dioxole-5-acetic acid

생성물 1

HCID 266588Methyl 2-(1,3-dioxaindan-5-yl)acetate수율 87.6%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

A mixture of (3,4-methylenedioxyphenyl)acetic acid (4.64 g, 25.74 mmol) in dry DMF (40 mL), cesium carbonate (9.2 g, 25.74 mmol) and methyl iodide (3.7 g, 26.0 mmol) in dry DMF (40 mL) was stirred at room temperature for 3h. At the end of this period, the reaction mixture was poured into ice water and extracted with ethyl acetate. The organic phase was washed with saturated NaHCO3, water, brine and then dried (MgSO4) and filtered. The filtrate was concentrated in vacuo to provide pure methyl (3,4-methylenedioxyphenyl)acetate as an oil (4.38 g).

후처리

  1. extractionextracted with ethyl acetate
  2. washThe organic phase was washed with saturated NaHCO3, water, brine
  3. dry with materialdried (MgSO4)
  4. filtrationfiltered
  5. concentrationThe filtrate was concentrated in vacuo

출처 및 근거

ORD 기록
ord-65362d73281c489fac77eb543a1e8af0
출처 데이터셋
uspto-grants-1995_02
특허 번호
US05391566

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