7-(3-Chloropropyl)-3,7-dihydro-1,3-dimethyl-1H-purine-2,6-dione → Fluprophylline

HRID 746253

反応式

HRID 746253 の反応式
[F:1][C:2]1[CH:15]=[CH:14][C:5]([C:6]([CH:8]2[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]2)=[O:7])=[CH:4][CH:3]=1.Cl[CH2:17][CH2:18][CH2:19][N:20]1[C:29]2[C:28](=[O:30])[N:26]([CH3:27])[C:25](=[O:31])[N:24]([CH3:32])[C:23]=2[N:22]=[CH:21]1>>[F:1][C:2]1[CH:3]=[CH:4][C:5]([C:6]([CH:8]2[CH2:13][CH2:12][N:11]([CH2:17][CH2:18][CH2:19][N:20]3[C:29]4[C:28](=[O:30])[N:26]([CH3:27])[C:25](=[O:31])[N:24]([CH3:32])[C:23]=4[N:22]=[CH:21]3)[CH2:10][CH2:9]2)=[O:7])=[CH:14][CH:15]=1

参加物

3

反応物 2

HCID 760117-(3-Chloropropyl)-3,7-dihydro-1,3-dimethyl-1H-purine-2,6-dioneHCID 27244404-(4-Fluorobenzoyl)piperidine

生成物 1

HCID 65636Fluprophylline収率 43.5%

反応条件

温度
100 °C

実験手順

10.2 g 4-(p-fluorobenzoyl)-piperidine and 16.5 g 7-(chloropropyl)-theophylline are carefully mixed in the solid state and heated to 100° C. in a round flask in an oil bath. The mixture at first results in a clear melt, subsequently begins to crystallize and then changes into a solid mass. It is allowed to cool after 10 minutes, dissolved in ethyl acetate and 2n hydrochloric acid is added, whereby a dark oil separates in the organic phase, crystallizing on standing overnight. By recrystallizaing with 100 ml carbon tetrachloride, an intially oily then crystallizing substance is obtained, 7.4 g of the product with an mp of 114° to 119° C. (yield: 43.5%)

後処理

  1. customThe mixture at first results in a clear melt
  2. customto crystallize
  3. temperatureto cool after 10 minutes
  4. dissolutiondissolved in ethyl acetate
  5. addition2n hydrochloric acid is added
  6. customwhereby a dark oil separates in the organic phase, crystallizing
  7. customan intially oily then crystallizing substance
  8. customis obtained

出典と根拠

ORDレコード
ord-46fa03f011a9453eb7129e6b18ed5bdc
出典データセット
uspto-grants-1986_07
特許番号
US04603204

関連ノート

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