Hexamethylenetetramine → 4-(2',6'-Dichlorobenzyl)oxazole

HRID 325950노트

반응식

HRID 325950 반응식
[Cl:1][C:2]1[CH:12]=[CH:11][CH:10]=[C:9]([Cl:13])[C:3]=1[CH2:4][C:5]([CH:7]=[O:8])=O.[CH2:14]1N2CN3CN(C2)C[N:15]1C3.C([O-])(=O)C.[NH4+]>C(N)=O>[Cl:1][C:2]1[CH:12]=[CH:11][CH:10]=[C:9]([Cl:13])[C:3]=1[CH2:4][C:5]1[N:15]=[CH:14][O:8][CH:7]=1

참가 물질

5

반응물 3

HCID 4101HexamethylenetetramineHCID 517165Ammonium AcetateHCID 204633232,6-Dichlorobenzylglyoxal

생성물 1

HCID 204633054-(2',6'-Dichlorobenzyl)oxazole

시약·촉매·용매 1

HCID 713Formamide용매

반응 조건

온도
100 °C

실험 절차

21.7 g of crude 2,6-dichlorobenzylglyoxal are dissolved in 50 ml of formamide. 7.0 g of hexamethylenetetramine and 30.8 g of ammonium acetate are added and the reaction mixture is stirred at 100° C. for 2 hours, then is evaporated to dryness in vacuo. 200 ml of water are added and the pH of the aqueous phase is adjusted, while stirring, to 2-3 with concentrate hydrochloric acid. The solution is washed with toluene (3×50 ml). The aqueous solution is made alkaline with sodium hydroxide (pH=8-9) and then extracted three times with chloroform (1×100 ml and 2×50 ml). The combined chloroform extracts are washed with water, dried with sodium sulfate and evaporated to dryness. The residue, which consisted of crude product, is used in step (c) below.

후처리

  1. customis evaporated to dryness in vacuo
  2. addition200 ml of water are added
  3. stirringwhile stirring, to 2-3 with concentrate hydrochloric acid
  4. washThe solution is washed with toluene (3×50 ml)
  5. extractionextracted three times with chloroform (1×100 ml and 2×50 ml)
  6. washThe combined chloroform extracts are washed with water
  7. dry with materialdried with sodium sulfate
  8. customevaporated to dryness

출처 및 근거

ORD 기록
ord-beaca45448a7416f9b2081a7557a3197
출처 데이터셋
uspto-grants-1984_04
특허 번호
US04443466

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