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Theobromine → HCID 20041114, 화합물

HRID 1762551
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HRID 1762551 반응식
[CH3:1][N:2]1[C:10]2[N:9]=[CH:8][N:7]([CH3:11])[C:6]=2[C:5](=[O:12])[NH:4][C:3]1=[O:13].Cl[CH2:15][CH2:16][CH2:17][CH:18]=[C:19]([CH3:21])[CH3:20].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[CH3:1][N:2]1[C:10]2[N:9]=[CH:8][N:7]([CH3:11])[C:6]=2[C:5](=[O:12])[N:4]([CH2:15][CH2:16][CH2:17][CH:18]=[C:19]([CH3:21])[CH3:20])[C:3]1=[O:13]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 5429TheobromineHCID 11430Potassium CarbonateHCID 133573926-Chloro-2-methylhex-2-ene

생성물 1

HCID 20041114HCID 20041114, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

9.0 g (0.05 mol) of 3,7-dimethylxanthine, 8.0 g (0.06 mol) of 1-chloro-5-methyl-4-hexene and 8.3 g (0.06 mol) of potassium carbonate are stirred in 200 ml of dimethylformamide at 110° C. for 22 hours. After the solvent has been removed in vacuo, 100 ml of 1N sodium hydroxide solution are added and the mixture is extracted thoroughly with methylene chloride. The extract is extracted again by shaking with dilute sodium hydroxide solution, washed with water until neutral, dried and evaporated under reduced pressure and the residue is recrystallized from diisopropyl ether.

후처리

  1. customAfter the solvent has been removed in vacuo, 100 ml of 1N sodium hydroxide solution
  2. additionare added
  3. extractionthe mixture is extracted thoroughly with methylene chloride
  4. extractionThe extract is extracted again
  5. washwashed with water until neutral,
  6. customdried
  7. customevaporated under reduced pressure
  8. customthe residue is recrystallized from diisopropyl ether

출처 및 근거

ORD 기록
ord-52f373a3bdbb44d9b9796d537f485edf
출처 데이터셋
uspto-grants-1989_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04833146

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