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Methyl iodide → 2-Methoxymethylene-3,3-dimethyl-indan-1-one

HRID 495117
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HRID 495117 반응식
[CH2:1]([O:3][CH:4]=O)[CH3:2].[H-].[Na+].C[C:9]1(C)[CH2:17][C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[C:10]1=[O:18].[CH3:20]I>C1COCC1>[CH3:4][O:3][CH:1]=[C:2]1[C:17]([CH3:9])([CH3:20])[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[C:10]1=[O:18]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 6328Methyl iodideHCID 8025Ethyl formateHCID 24758Sodium hydrideHCID 3012022,2-dimethyl-2,3-dihydro-1H-inden-1-one

생성물 1

HCID 686158752-Methoxymethylene-3,3-dimethyl-indan-1-one

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매3회

실험 절차

Ethylformate (8.10 g, 110 mmol) in THF (50 ml) was added to the suspension of NaH (55% in mineral oil, 4.80 g, 110 mmol) in THF (50 ml). After stirring for 5 min at RT Dimethylindanone (16.0 g, 100 mmol)in THF (50 ml) was added. Gas evolution started and the temperature of the mixture rose and was controlled with an icebath to not exceed 40° C. After further stirring for 4.5 h at RT, methyl iodide (42.6 g, 300 mmol) was added und stirring continued for 48 h. After quenching with aq. NaHCO3-solution and aqueous workup a dark red oil (20.4 g, 100%) of was obtained.

후처리

  1. additionwas added
  2. customexceed 40° C
  3. stirringund stirring
  4. waitcontinued for 48 h
  5. customAfter quenching with aq. NaHCO3-solution and aqueous workup a dark red oil (20.4 g, 100%)
  6. customof was obtained

출처 및 근거

ORD 기록
ord-582895f1e2c74c1c9a827abc7c7859eb
출처 데이터셋
uspto-grants-2009_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07538243B2

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