Water → HCID 53739414, 화합물

HRID 1706377

반응식

HRID 1706377 반응식
[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]

참가 물질

7

반응물 4

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

생성물 1

HCID 53739414HCID 53739414, 화합물

시약·촉매·용매 2

HCID 1140Toluene용매HCID 3283Diethyl Ether용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ae92d91a65bc45d7af021acff4dc034d
출처 데이터셋
uspto-grants-1980_06
특허 번호
US04207321

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