Hydrochloric Acid → HCID 13112734、化合物

HRID 1764443

反応式

HRID 1764443 の反応式
[NH2:1][C:2]1[N:7]=[C:6]([NH2:8])[C:5]([CH2:9]O)=[CH:4][N:3]=1.[CH2:11]([C:13]1[CH:18]=[CH:17][CH:16]=[C:15]([CH2:19][CH3:20])[C:14]=1[OH:21])[CH3:12].Cl>C1(C)C=CC(S(O)(=O)=O)=CC=1.CCOCC>[NH2:1][C:2]1[N:7]=[C:6]([NH2:8])[C:5]([CH2:9][C:17]2[CH:16]=[C:15]([CH2:19][CH3:20])[C:14]([OH:21])=[C:13]([CH2:11][CH3:12])[CH:18]=2)=[CH:4][N:3]=1

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 705072,6-DiethylphenolHCID 2958782,4-Diamino-5-pyrimidinemethanol

生成物 1

HCID 13112734HCID 13112734、化合物

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 6101p-Toluenesulfonic acid溶媒

実験手順

2,4-Diamino-5-hydroxymethylpyrimidine (1.4 g.), prepared as in Example 1, and 2,6-diethylphenol (1.6 g.) in toluene-4-sulphonic acid (10 g.) containing conc. hydrochloric acid (3 ml.) were heated on the steam-bath for 6 hours. The solution was cooled, diluted with ether and the ether decanted. The residue was treated with a soln. of sodium hydrogen carbonate and the solid filtered off. Recrystallisation from aqueous ethanol gave colourless needles of 2,4-diamino-5-(3,5-diethyl-4-hydroxybenzyl)pyrimidine, m.p. 200°-202° C.

後処理

  1. temperaturewere heated on the steam-bath for 6 hours
  2. temperatureThe solution was cooled
  3. customthe ether decanted
  4. additionThe residue was treated with a soln
  5. filtrationof sodium hydrogen carbonate and the solid filtered off
  6. customRecrystallisation from aqueous ethanol

出典と根拠

ORDレコード
ord-0b7399da98c14c6ea6e0eeb4d684da5e
出典データセット
uspto-grants-1978_09
特許番号
US04116958

関連ノート

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