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Potassium Carbonate → HCID 20544126, 화합물

HRID 2285784
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HRID 2285784 반응식
Cl[CH2:2][CH:3]1[CH2:7][N:6]([CH:8]([CH3:10])[CH3:9])[C:5](=[O:11])[C:4]1([C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.[Cl:24][C:25]1[CH:30]=[CH:29][C:28]([C:31]2([OH:37])[CH2:36][CH2:35][NH:34][CH2:33][CH2:32]2)=[CH:27][CH:26]=1.[C:38](=[O:41])([O-:40])[O-].[K+].[K+]>C(O)C>[OH2:11].[C:5]([OH:11])(=[O:37])[C:38]([OH:40])=[O:41].[Cl:24][C:25]1[CH:30]=[CH:29][C:28]([C:31]2([OH:37])[CH2:32][CH2:33][N:34]([CH2:2][CH:3]3[CH2:7][N:6]([CH:8]([CH3:9])[CH3:10])[C:5](=[O:11])[C:4]3([C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)[C:12]3[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=3)[CH2:35][CH2:36]2)=[CH:27][CH:26]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 382824-(4-Chlorophenyl)-4-hydroxypiperidineHCID 12953546HCID 12953546, 화합물

생성물 1

HCID 20544126HCID 20544126, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 18 g. (0.06 mole) of 4-chloromethyl-1-(1-methylethyl)-3,3-diphenyl-2-pyrrolidinone, 11.6 g. (0.06 mole) of 4-(4-chlorophenyl)-4-hydroxypiperidine and 20 g. (0.14 mole) potassium carbonate in 200 ml. of ethanol was heated to 200° C. for 48 hrs. in a steel bomb. During the heating the bomb was continuously rotated to produce mild stirring. The mixture was concentrated and the residue partitioned between chloroform sodium hydroxide. The chloroform was dried (sodium sulfate) and concentrated. The residue was dissolved in ethyl-acetate and treated with ethereal hydrogen chloride. The mixture was filtered and the filtrate extracted with water. The acid layer was made basic with dilute sodium hydroxide and extracted with chloroform which was dried (sodium sulfate) and concentrated. The residue was dissolved in isopropyl alcohol and treated with oxalic acid. The resulting crystals were recrystallized from ethanol-water. The product (3 g., 10%) melted at 240° C. (dec.).

후처리

  1. additionA mixture of 18 g
  2. customto produce mild stirring
  3. concentrationThe mixture was concentrated
  4. customthe residue partitioned between chloroform sodium hydroxide
  5. dry with materialThe chloroform was dried (sodium sulfate)
  6. concentrationconcentrated
  7. dissolutionThe residue was dissolved in ethyl-acetate
  8. additiontreated with ethereal hydrogen chloride
  9. filtrationThe mixture was filtered
  10. extractionthe filtrate extracted with water
  11. extractionextracted with chloroform which
  12. dry with materialwas dried (sodium sulfate)
  13. concentrationconcentrated
  14. dissolutionThe residue was dissolved in isopropyl alcohol
  15. additiontreated with oxalic acid
  16. customThe resulting crystals were recrystallized from ethanol-water

출처 및 근거

ORD 기록
ord-b3ea8cda7650459195cae8e846086d51
출처 데이터셋
uspto-grants-1982_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04324791

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