Hydrochloric Acid → HCID 178516872, 화합물

HRID 483314

반응식

HRID 483314 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]2[CH2:13][CH2:12][CH:11]([C:14]3[C:15](=[O:26])[C:16]4[C:21]([C:22](=[O:25])[C:23]=3Cl)=[CH:20][CH:19]=[CH:18][CH:17]=4)[CH2:10][CH2:9]2)=[CH:4][CH:3]=1.[OH-:27].[K+].Cl>CO.O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([CH:8]2[CH2:9][CH2:10][CH:11]([C:14]3[C:15](=[O:26])[C:16]4[C:21]([C:22](=[O:25])[C:23]=3[OH:27])=[CH:20][CH:19]=[CH:18][CH:17]=4)[CH2:12][CH2:13]2)=[CH:6][CH:7]=1

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 111010701,4-Naphthalenedione, 2-chloro-3-[cis-4-(4-chlorophenyl)cyclohexyl]-

생성물 1

HCID 178516872HCID 178516872, 화합물

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

The product of stage (b) was suspended in 10 ml of boiling methanol and 0.55 g of potassium hydroxide in 5.5 ml of water was added dropwise over 15 mins. The mixture was refluxed until a dark red solution formed, (after ca. 6 hrs) when 2 ml of concentrated hydrochloric acid was cautiously added dropwise. The mixture was cooled and filtered, and the solid residue washed thoroughly with water. The water washings were re-acidified and filtered. The combined solid residues (500 mg) mp 200°-209°, were recrystallised from acetonitrile to give the title product as the trans-isomer (300 mg) m.p. 216°-219° C.

후처리

  1. temperatureThe mixture was refluxed until a dark red solution
  2. customformed
  3. temperatureThe mixture was cooled
  4. filtrationfiltered
  5. washthe solid residue washed thoroughly with water
  6. filtrationfiltered
  7. customThe combined solid residues (500 mg) mp 200°-209°, were recrystallised from acetonitrile

출처 및 근거

ORD 기록
ord-2dc73421b5874c808cbcb150b19206c6
출처 데이터셋
uspto-grants-1993_07
특허 번호
US05225184

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