Water → HCID 53739414、化合物

HRID 1706377

反応式

HRID 1706377 の反応式
[CH3:1][N:2]1[C:11](=[O:12])[C:10]2[N:9]([CH2:13][CH2:14][CH2:15][CH2:16][CH:17](O)[CH3:18])[CH:8]=[N:7][C:6]=2[N:5]([CH3:20])[C:3]1=[O:4].C1(C)C=CC(S(O)(=O)=O)=CC=1.O.CN1C(=O)C2N(CCCCC=C)C=NC=2N(C)C1=O>C1(C)C=CC=CC=1.C(OCC)C>[CH3:1][N:2]1[C:11](=[O:12])[C:10]2[N:9]([CH2:13][CH2:14][CH2:15][CH:16]=[CH:17][CH3:18])[CH:8]=[N:7][C:6]=2[N:5]([CH3:20])[C:3]1=[O:4]

参加物

7

反応物 4

HCID 962WaterHCID 6101p-Toluenesulfonic acidHCID 12807387HCID 12807387、化合物HCID 150526747-(5-Hydroxyhexyl)-1,3-dimethylxanthine

生成物 1

HCID 53739414HCID 53739414、化合物

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 3283Diethyl Ether溶媒

実験手順

7 g of 1,3-dimethyl-7-(5-hydroxyhexyl)-xanthine and 9.5 g of p-toluene sulphonic acid are refluxed in 100 ml of toluene for 12 hours with continuous separation of the water formed in the reaction. After cooling to room temperature, the reaction mixture is mixed with 100 ml of diethyl ether, washed with sodium bicarbonate solution and water until neutral and the organic phase dried over sodium sulphate is evaporated under reduced pressure. After column chromatography on silica gel with methylene chloride/acetone (1:1) as eluent and distillation under reduced pressure a product is obtained from the residue which still contains a few percent of isomeric 1,3-dimethyl-7-(hex-5-enyl)-xanthine (as shown by the n.m.r. spectrum). Yield: 4.3 g (65.5% of theory relative to the starting product used). Melting point: 58°-64° C.

後処理

  1. customformed in the reaction
  2. washwashed with sodium bicarbonate solution and water until neutral and the organic phase
  3. dry with materialdried over sodium sulphate
  4. customis evaporated under reduced pressure
  5. distillationAfter column chromatography on silica gel with methylene chloride/acetone (1:1) as eluent and distillation under reduced pressure a product
  6. customis obtained from the residue which

出典と根拠

ORDレコード
ord-ae92d91a65bc45d7af021acff4dc034d
出典データセット
uspto-grants-1980_06
特許番号
US04207321

関連ノート

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