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

HRID 2092242

반응식

HRID 2092242 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 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.

후처리

  1. temperaturethe reaction mixture is heated
  2. temperatureat reflux for 30 min
  3. extractionThe mixture is extracted three times with in each case 20 ml of ethyl acetate
  4. washThe combined organic phases are washed twice with in each case 5 ml of water
  5. dry with materialdried over magnesium sulfate
  6. customThe solvent is removed on a rotary evaporator
  7. customThe residue is used without further purification in the subsequent steps

출처 및 근거

ORD 기록
ord-7ca0568187df40849803db9f8eea639d
출처 데이터셋
uspto-grants-2013_05
특허 번호
US08440700B2

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