Allylamine → HCID 18326381、化合物

HRID 1250626

反応式

HRID 1250626 の反応式
[CH2:1]([N:4]([CH2:16][CH:17]=[CH2:18])[C:5]1[C:6]2[S:14][CH:13]=[C:12]([CH3:15])[C:7]=2[N:8]=[C:9]([Cl:11])[N:10]=1)[CH:2]=[CH2:3].[CH2:19]([NH2:22])[CH:20]=[CH2:21].C(=O)([O-])O.[Na+]>>[ClH:11].[CH2:19]([NH:22][C:9]1[N:10]=[C:5]([N:4]([CH2:16][CH:17]=[CH2:18])[CH2:1][CH:2]=[CH2:3])[C:6]2[S:14][CH:13]=[C:12]([CH3:15])[C:7]=2[N:8]=1)[CH:20]=[CH2:21]

参加物

4

反応物 3

HCID 7853AllylamineHCID 516892Sodium BicarbonateHCID 183265134-Diallylamino-2-chloro-7-methylthieno[3,2-d]pyrimidine

生成物 1

HCID 18326381HCID 18326381、化合物

実験手順

In a sealed tube were heated 335 mg (1.2 mmol) of 4-diallylamino-2-chloro-7-methylthieno[3,2-d]pyrimidine and 1.10 g (19.2 mmol) of allylamine at 140° C. for 16 hours. After completion of the reaction, the reaction mixture was allowed to resume room temperature, and a saturated aqueous sodium hydrogen carbonate solution was added thereto, followed by extraction with ethyl acetate (50 ml×2). The organic layer was washed with brine and dried over anhydrous sodium sulfate, and then the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (eluent: ethyl acetate-hexane=1/4) to give 277 mg (yield: 77.0%) of a free base compound of the title compound.

後処理

  1. customAfter completion of the reaction
  2. customto resume room temperature
  3. extractionfollowed by extraction with ethyl acetate (50 ml×2)
  4. washThe organic layer was washed with brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. distillationthe solvent was distilled off under reduced pressure
  7. customThe residue was purified by silica gel column chromatography (eluent: ethyl acetate-hexane=1/4)

出典と根拠

ORDレコード
ord-d2f5b77e193f40aa827759bc873706ba
出典データセット
uspto-grants-2002_01
特許番号
US06339089B2

関連ノート

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