Potassium Hydroxide → HCID 70982700, 화합물

HRID 922616노트

반응식

HRID 922616 반응식
[Cl:1][C:2]1[N:3]=[CH:4][NH:5][C:6]=1[Cl:7].[OH-].[K+].Br[CH2:11][C:12]1[CH:25]=[CH:24][C:23]2[C:22](=[O:26])[C:21]3[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=3)[C:15](=[O:27])[C:14]=2[CH:13]=1>C(#N)C>[CH3:11][C:12]1[CH:25]=[CH:24][C:23]2[C:22](=[O:26])[C:21]3[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=3)[C:15](=[O:27])[C:14]=2[C:13]=1[N:3]1[C:2]([Cl:1])=[C:6]([Cl:7])[N:5]=[CH:4]1

참가 물질

5

반응물 3

HCID 14797Potassium HydroxideHCID 1400184,5-DichloroimidazoleHCID 3444522-Bromomethyl-anthraquinone2회

생성물 1

HCID 70982700HCID 70982700, 화합물수율 40%

시약·촉매·용매 1

HCID 6342Acetonitrile용매2회

실험 절차

4,5-Dichloroimidazole (0.18 g, 1.33 mmol) and potassium hydroxide (0.08 g, 1.46 mmol) were combined in a round bottom flask. Acetonitrile (2 mL) was added and the mixture was stirred at reflux for 30 min, dissolving the remaining solid. Concurrently, 2-(Bromomethyl)anthraquinone (0.4 g, 1.33 mmol) was added to 30 mL acetonitrile and stirred at reflux for 30 min, partially dissolving the solid. The solution in the initial flask was added to the 2-(bromomethyl)anthraquinone mixture, and the solution was returned to reflux for 3 h. The mixture was filtered hot, and a precipitate quickly formed in the tan filtrate. The precipitate was collected by a second filtration and washed with cold acetonitrile to yield a yellow powder (0.19 g, 40% yield). 1H NMR (300 MHz, DMSO-d6) 8.20 (3H, m, Ar), 8.10 (1H, s, NCHN), 8.01 (1H, d, Ar), 7.89-7.95 (2H, m, Ar), 7.74 (1H, dd, Ar), 5.51 (2H, s, CH2).

후처리

  1. temperatureat reflux for 30 min
  2. dissolutiondissolving the remaining solid
  3. stirringstirred
  4. temperatureat reflux for 30 min
  5. dissolutionpartially dissolving the solid
  6. temperatureto reflux for 3 h
  7. filtrationThe mixture was filtered hot
  8. customa precipitate quickly formed in the tan filtrate
  9. filtrationThe precipitate was collected by a second filtration
  10. washwashed with cold acetonitrile

출처 및 근거

ORD 기록
ord-691f1dfd8ff243a08b1cec51137620ba
출처 데이터셋
uspto-grants-2016_03
특허 번호
US09278951B2

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