7-(2-Chloroethyl)theophylline → HCID 13534156, 화합물

HRID 464649노트

반응식

HRID 464649 반응식
Cl[CH2:2][CH2:3][N:4]1[C:12]2[C:11](=[O:13])[N:10]([CH3:14])[C:9](=[O:15])[N:8]([CH3:16])[C:7]=2[N:6]=[CH:5]1.[NH:17]1[CH2:22][CH2:21][CH:20]([C:23]2[C:31]3[C:26](=[CH:27][CH:28]=[C:29]([OH:32])[CH:30]=3)[NH:25][CH:24]=2)[CH2:19][CH2:18]1.C(=O)([O-])[O-].[Na+].[Na+].[I-].[K+]>CC(C)CC(=O)C>[OH:32][C:29]1[CH:30]=[C:31]2[C:26](=[CH:27][CH:28]=1)[NH:25][CH:24]=[C:23]2[CH:20]1[CH2:21][CH2:22][N:17]([CH2:2][CH2:3][N:4]2[C:12]3[C:11](=[O:13])[N:10]([CH3:14])[C:9](=[O:15])[N:8]([CH3:16])[C:7]=3[N:6]=[CH:5]2)[CH2:18][CH2:19]1

참가 물질

6

반응물 4

HCID 18827-(2-Chloroethyl)theophyllineHCID 4875Potassium IodideHCID 10340Sodium CarbonateHCID 122292493-(4-piperidinyl)-1H-indol-5-ol

생성물 1

HCID 13534156HCID 13534156, 화합물수율 43%

시약·촉매·용매 1

HCID 7909Methyl Isobutyl Ketone용매

실험 절차

A mixture of 3.65 parts of 7-(2-chloroethyl)-3,7-dihydro-1,3-dimethyl-1H-purine-2,6-dione, 3 parts of 3-(4-piperidinyl)-1H-indol-5-ol, 4.25 parts of sodium carbonate, 0.1 parts and potassium iodide and 200 parts of 4-methyl-2-pentanone was stirred and refluxed overnight. The whole was filtered while hot and the filtrate was evaporated. The residue was suspended in 45 parts of trichloromethane and 2.4 parts of methanol. The product was filtered off, washed with 16 parts of methanol and dried, yielding 2.5 parts (43%) of 3,7-dihydro-7-[2-[4-(5-hydroxy-1H-indol-3-yl)-1-piperidinyl]ethyl]-1,3-dimethyl-1H-purine-2,6-dione; mp. 232.5° C. (compound 2).

후처리

  1. temperaturerefluxed overnight
  2. filtrationThe whole was filtered while hot and the filtrate
  3. customwas evaporated
  4. filtrationThe product was filtered off
  5. washwashed with 16 parts of methanol
  6. customdried

출처 및 근거

ORD 기록
ord-b1feb3073dc8466e92857eab1695ff2f
출처 데이터셋
uspto-grants-1985_10
특허 번호
US04548939

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