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

HRID 508162

反応式

HRID 508162 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

反応条件

温度
0 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-867345793a3c4a99be0f169b1582f752
出典データセット
uspto-grants-2015_08
特許番号
US09095582B2

関連ノート

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