참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Ammonia | HCID 222 | — |
| 반응물 | Phosphorus oxychloride | HCID 24813 | — |
| 반응물 | 2-(4-Chlorophenyl)-4,5-dimethyl-1,3-oxazol 3-oxide | HCID 3243952 | — |
| 용매 | Chloroform | HCID 6212 | — |
| 생성물 | 4-(Chloromethyl)-2-(4-chlorophenyl)-5-methyl-1,3-oxazole | HCID 3613658 | — |
반응 단계
1.00 g (4.47 mmol) of the compound from Example 31A are initially charged in 15 ml of chloroform, and 1.5 ml (16.10 mmol) of phosphoryl chloride are added carefully. With stirring, the reaction mixture is heated at reflux for 30 min. The mixture is then cooled to 0° C. and made weakly basic by addition of ammonia. The mixture is extracted three times with in each case 20 ml of ethyl acetate. The combined organic phases are washed twice with in each case 5 ml of water and then dried over magnesium sulfate. The solvent is removed on a rotary evaporator. The residue is used without further purification in the subsequent steps.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09095582B2 |
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| 출처 데이터셋 | uspto-grants-2015_08 |
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| ORD ID | ord-867345793a3c4a99be0f169b1582f752 |
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| 출처 메모 | uspto-grants-2015_08 |
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