BAY-i 9139 → HCID 21320003, 화합물

HRID 262106

반응식

HRID 262106 반응식
[Cl:1][C:2]1[CH:20]=[CH:19][C:5]([O:6][CH:7]([N:14]2[CH:18]=[CH:17][N:16]=[CH:15]2)[CH:8]([OH:13])[C:9]([CH3:12])([CH3:11])[CH3:10])=[CH:4][CH:3]=1.[C:21]([O-])(=[O:23])[CH3:22].[Na+]>C(OC(=O)C)(=O)C>[C:21]([O:13][CH:8]([C:9]([CH3:11])([CH3:12])[CH3:10])[CH:7]([O:6][C:5]1[CH:4]=[CH:3][C:2]([Cl:1])=[CH:20][CH:19]=1)[N:14]1[CH:18]=[CH:17][N:16]=[CH:15]1)(=[O:23])[CH3:22]

참가 물질

4

반응물 2

HCID 171440BAY-i 9139HCID 517045Sodium Acetate

생성물 1

HCID 21320003HCID 21320003, 화합물수율 730.7%

시약·촉매·용매 1

HCID 7918Acetic Anhydride용매

실험 절차

8.0 g (0.027 mol) of 1-(4-chlorophenoxy)-1-imidazol-1-yl-3,3-dimethyl-butan-2-ol are heated in 40 ml of acetic anhydride with 0.15 g of sodium acetate for 10 hours at 100° C. The solution is then cooled and stirred into 400 ml of ice water, the temperature being kept at 20°-25° C. The mixture is left to stand overnight. A smeary crystalline mass precipitates out and is taken up in chloroform. The chloroform solution is washed several times with water and sodium bicarbonate solution, dried over sodium sulphate and concentrated in vacuo by distilling off the solvent. The crystalline residue is boiled up in petroleum ether and the product is filtered off cold and dried. 4.5 g (49% of theory) of 2-acetoxy-1-(4-chlorophenoxy)-1-imidazol-1-yl-3,3-dimethylbutane are obtained as a mixture of isomers with a melting point of 81°-91° C.

후처리

  1. temperatureThe solution is then cooled
  2. custombeing kept at 20°-25° C
  3. waitThe mixture is left
  4. customA smeary crystalline mass precipitates out and
  5. washThe chloroform solution is washed several times with water and sodium bicarbonate solution
  6. dry with materialdried over sodium sulphate
  7. concentrationconcentrated in vacuo
  8. distillationby distilling off the solvent
  9. filtrationthe product is filtered off cold
  10. customdried

출처 및 근거

ORD 기록
ord-72602ba60b2c4a35b8b62dca1152f608
출처 데이터셋
uspto-grants-1979_05
특허 번호
US04153692

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