참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Methane, dichloromethoxy- | HCID 21004 | — |
| 반응물 | Methyl 2-methyl-2-phenylpropanoate | HCID 143498 | — |
| 촉매 | Titanium Tetrachloride | HCID 24193 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | HCID 25111210 | HCID 25111210 | 63.8% |
반응 단계
6.80 g (38 mmol) of 2-methyl-2-phenyl-propionic acid methyl ester was dissolved at rt in 200 mL MeCl2 and 7.01 ml (90.4 g=76 mmol) of dichloromethylmethylether was added and the mixture cooled down to 0° C.; 21.47 mL (36.93 g=191 mmol) TiCl4 was added over 15 min and the reaction warmed up to ambient temperature; stirring was continued for 16 hours. The reaction mixture was then treated at 0° C. with 20 ml of HCl (37% in water) and extracted twice with MeCl2; the organic phases were washed with water, dried over MgSO4, filtered and evaporated. The crude product was purified by chromatography (silicagel, eluent:gradient of n-heptane/EtOAc) to yield 5.00 g of the title compound as yellow oil. MS: 206.1 (M+).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07772253B2 |
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| 출처 데이터셋 | uspto-grants-2010_08 |
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| ORD ID | ord-5cc4fa502e1a4abf8341995c0ee1255f |
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| 출처 메모 | uspto-grants-2010_08 |
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