BAY-i 9139 → HCID 21320003、化合物

HRID 262106

反応式

HRID 262106 の反応式
[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]

参加物

4

反応物 2

HCID 171440BAY-i 9139HCID 517045Sodium Acetate

生成物 1

HCID 21320003HCID 21320003、化合物収率 730.7%

試薬・触媒・溶媒 1

HCID 7918Acetic Anhydride溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-72602ba60b2c4a35b8b62dca1152f608
出典データセット
uspto-grants-1979_05
特許番号
US04153692

関連ノート

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