Ammonia → 4-(Chloromethyl)-2-(4-chlorophenyl)-5-methyl-1,3-oxazole

HRID 1916262

반응식

HRID 1916262 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[O:9][C:10]([CH3:15])=[C:11]([CH3:14])[N+:12]=2[O-])=[CH:4][CH:3]=1.P(Cl)(Cl)([Cl:18])=O.N>C(Cl)(Cl)Cl>[Cl:18][CH2:14][C:11]1[N:12]=[C:8]([C:5]2[CH:6]=[CH:7][C:2]([Cl:1])=[CH:3][CH:4]=2)[O:9][C:10]=1[CH3:15]

참가 물질

5

반응물 3

HCID 222AmmoniaHCID 24813Phosphorus oxychlorideHCID 32439522-(4-Chlorophenyl)-4,5-dimethyl-1,3-oxazol 3-oxide

생성물 1

HCID 36136584-(Chloromethyl)-2-(4-chlorophenyl)-5-methyl-1,3-oxazole

시약·촉매·용매 1

HCID 6212Chloroform용매

반응 조건

온도
0 °C

실험 절차

1.00 g (4.47 mmol) of the compound from Example 13A were initially charged in 15 ml of chloroform, and 1.5 ml (16.10 mmol) of phosphorus oxychloride were added carefully. With stirring, the reaction mixture was heated under reflux for 30 min. The reaction was then cooled to 0° C. and made slightly basic by addition of 25% strength aqueous ammonia solution. The mixture was extracted three times with in each case 20 ml of ethyl acetate. The combined organic phases were washed twice with in each case 5 ml of water and then dried over magnesium sulfate. The solvent was removed on a rotary evaporator. Without further purification, the residue was used for the subsequent steps.

후처리

  1. temperaturethe reaction mixture was heated
  2. temperatureunder reflux for 30 min
  3. extractionThe mixture was extracted three times with in each case 20 ml of ethyl acetate
  4. washThe combined organic phases were washed twice with in each case 5 ml of water
  5. dry with materialdried over magnesium sulfate
  6. customThe solvent was removed on a rotary evaporator
  7. customWithout further purification

출처 및 근거

ORD 기록
ord-962d86d60f4146a5b2ed0edd8944f1dd
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08618119B2

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