7-(2-Chloroethyl)theophylline → HCID 13534156、化合物

HRID 464649ノート

反応式

HRID 464649 の反応式
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

参加物

6

反応物 4

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

生成物 1

HCID 13534156HCID 13534156、化合物収率 43%

試薬・触媒・溶媒 1

HCID 7909Methyl Isobutyl Ketone溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-b1feb3073dc8466e92857eab1695ff2f
出典データセット
uspto-grants-1985_10
特許番号
US04548939

反応ノート

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