Hydrochloric Acid → HCID 21551717, 화합물

HRID 268215

반응식

HRID 268215 반응식
[N+:1]([C:4]1[CH:11]=[CH:10][CH:9]=[CH:8][C:5]=1[CH:6]=[O:7])([O-:3])=O.[CH3:12][CH:13]1[CH2:18][C:17](=[O:19])[CH2:16][C:15](=O)[CH2:14]1.[ClH:21].O>O1CCCC1>[Cl:21][C:9]1[CH:8]=[C:5]2[C:4]([N:1]([OH:3])[C:15]3[CH2:14][CH:13]([CH3:12])[CH2:18][C:17](=[O:19])[C:16]=3[C:6]2=[O:7])=[CH:11][CH:10]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 111012-NitrobenzaldehydeHCID 4580955-Methylcyclohexane-1,3-dione

생성물 1

HCID 21551717HCID 21551717, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

30.2 g (0.2 mole) of 2-nitrobezaldehyde and 25.2 g (0.2 mole) of 5-methyl-1,3-cyclohexane-dione were dissolved in 300 ml of tetrahydrofurane, the solution was saturated at 18° C with hydrogen chloride and allowed to stand for 4 days at room temperature. Water was added, the oily layer was separated and stirred with methanol. The crystals that had formed were filtered off, washed with methanol and dissolved and recrystallized from glacial acetic acid. 9.5 g (17 % of the theory) of 7-chloro-3-methyl-10-hydroxy-1-oxo-1,2,3,4-tetrahydro-9(10H)-acridone having a decomposition point of 255° C were obtained.

후처리

  1. customthe oily layer was separated
  2. customThe crystals that had formed
  3. filtrationwere filtered off
  4. washwashed with methanol
  5. dissolutiondissolved
  6. customrecrystallized from glacial acetic acid

출처 및 근거

ORD 기록
ord-b7b28e330e6243c899d66b4fb4eab0ff
출처 데이터셋
uspto-grants-1976_03
특허 번호
US03947449

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