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Water → 1-(3,4-Dimethoxyphenoxy)-3-[2-(1,3,5-trimethylpyrimidine-2,4-dion-6-ylamino)-ethylamino]-propan-2-ol

HRID 365179
ノート
印刷プレビュー

反応式

HRID 365179 の反応式
[CH2:1]([O:5][C:6]1[CH:11]=[CH:10][C:9]([O:12][CH3:13])=[C:8]([O:14][CH3:15])[CH:7]=1)[CH:2]1[O:4][CH2:3]1.[NH2:16][CH2:17][CH2:18][NH:19][C:20]1[N:21]([CH3:30])[C:22](=[O:29])[N:23]([CH3:28])[C:24](=[O:27])[C:25]=1[CH3:26].CN(C)C=O.O>C(Cl)Cl>[CH3:15][O:14][C:8]1[CH:7]=[C:6]([CH:11]=[CH:10][C:9]=1[O:12][CH3:13])[O:5][CH2:1][CH:2]([OH:4])[CH2:3][NH:16][CH2:17][CH2:18][NH:19][C:20]1[N:21]([CH3:30])[C:22](=[O:29])[N:23]([CH3:28])[C:24](=[O:27])[C:25]=1[CH3:26]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 6228DimethylformamideHCID 128188664-(2-aminoethylamino)-1,3,5-trimethylpyrimidine-2,6(1H,3H)-dioneHCID 202378293,4-Dimethoxyphenyl glycidyl ether

生成物 1

HCID 128188611-(3,4-Dimethoxyphenoxy)-3-[2-(1,3,5-trimethylpyrimidine-2,4-dion-6-ylamino)-ethylamino]-propan-2-ol

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒

実験手順

4.2 g. 3,4-Dimethoxyphenyl glycidyl ether and 8.5 g. 4-(2-aminoethylamino)-1,3,5-trimethylpyrimidine-2,6(1H,3H)-dione in 5 ml. dimethylformamide are left to stand for 48 hours at ambient temperature. The reaction mixture is then dissolved in methylene chloride, shaken out five times with water and the organic phase is extracted with 1N acetic acid. The aqueous phase is rendered alkaline by the addition of dilute aqueous sodium hydroxide solution and then extracted with methylene chloride. After drying the extract, the solution is chromatographed over silica gel using, as elution agent, methylene chloride-methanol-ammoniacal methanol (saturated) (20:1:1 v/v/v). After evaporating the pure fractions, the residue obtained is recrystallized from ethyl acetate. There are obtained 2.0 g. (24% of theory) of the desired product in the form of colorless crystals; m.p. 103°-104° C.

後処理

  1. extractionthe organic phase is extracted with 1N acetic acid
  2. additionby the addition of dilute aqueous sodium hydroxide solution
  3. extractionextracted with methylene chloride
  4. customAfter drying the extract
  5. customthe solution is chromatographed over silica gel using, as elution agent, methylene chloride-methanol-ammoniacal methanol (saturated) (20:1:1 v/v/v)
  6. customAfter evaporating the pure fractions
  7. customthe residue obtained
  8. customis recrystallized from ethyl acetate
  9. customThere are obtained 2.0 g

出典と根拠

ORDレコード
ord-29a35655462641bda172df2c5863c2cf
出典データセット
uspto-grants-1986_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04608383

反応ノート

読み込み中…

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