三氯生 → 5-Chloro-2-(2,4-dichlorophenoxy)phenyl 4-carboxy-2,2-dimethylbutyrate

HRID 279911

反应方程式

HRID 279911 反应方程式
[CH:1]1[C:6]([Cl:7])=[CH:5][C:4]([OH:8])=[C:3]([O:9][C:10]2[CH:11]=[CH:12][C:13]([Cl:17])=[CH:14][C:15]=2[Cl:16])[CH:2]=1.[CH3:18][C:19]1([CH3:27])[CH2:25][CH2:24][C:23](=[O:26])[O:22][C:20]1=[O:21]>C(N(CC)CC)C>[C:23]([CH2:24][CH2:25][C:19]([CH3:27])([CH3:18])[C:20]([O:8][C:4]1[CH:5]=[C:6]([Cl:7])[CH:1]=[CH:2][C:3]=1[O:9][C:10]1[CH:11]=[CH:12][C:13]([Cl:17])=[CH:14][C:15]=1[Cl:16])=[O:21])([OH:26])=[O:22]

参与物

4

反应物 2

HCID 5564三氯生HCID 762472,2-二甲基戊二酸酐

产物 1

HCID 233229055-Chloro-2-(2,4-dichlorophenoxy)phenyl 4-carboxy-2,2-dimethylbutyrate

试剂、催化剂与溶剂 1

HCID 8471三乙胺溶剂2 次

反应条件

温度
80 °C

实验过程

A mixture of triclosan (29.0 g.), triethylamine (15 ml.) and 2,2-dimethylglutaric anhydride (20 g.) was heated at 80° C. for 5 hours. A further quantity (2.0 g.) of anhydride and triethylamine (1 ml.) were added and heating continued for 24 hours. The mixture was cooled to ambient temperature, washed with 2M hydrochloric acid (100 ml.), then with water (3×80 ml.) and dried (MgSO4). The solution obtained was evaporated. The brown residual oil was dissolved in hot cyclohexane. The solution on cooling gave white crystals which were recrystallised from cyclohexane/petrol 60-80 to give 5-chloro-2-(2,4-dichlorophenoxy)phenyl 4-carboxy-2,2-dimethylbutyrate (C') (12.7 g.), m.p. 125°-128° C.

后处理

  1. temperatureheating
  2. temperatureThe mixture was cooled to ambient temperature
  3. washwashed with 2M hydrochloric acid (100 ml.)
  4. dry with materialwith water (3×80 ml.) and dried (MgSO4)
  5. customThe solution obtained
  6. customwas evaporated
  7. dissolutionThe brown residual oil was dissolved in hot cyclohexane
  8. temperatureThe solution on cooling
  9. customgave white crystals which
  10. customwere recrystallised from cyclohexane/petrol 60-80

来源与证据

ORD记录
ord-d097fe9abe56492db156157af1bcf77c
来源数据集
uspto-grants-1986_05
专利号
US04587262

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