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Allylamine → HCID 18326466、化合物

HRID 1250677
ノート
印刷プレビュー

反応式

HRID 1250677 の反応式
[CH2:1]([NH:4][C:5]1[C:6]2[S:14][CH:13]=[C:12]([CH2:15][CH2:16][CH3:17])[C:7]=2[N:8]=[C:9](Cl)[N:10]=1)[CH:2]=[CH2:3].[CH2:18]([NH2:21])[CH:19]=[CH2:20].C(=O)([O-])O.[Na+]>>[CH2:18]([NH:21][C:9]1[N:10]=[C:5]([NH:4][CH2:1][CH:2]=[CH2:3])[C:6]2[S:14][CH:13]=[C:12]([CH2:15][CH2:16][CH3:17])[C:7]=2[N:8]=1)[CH:19]=[CH2:20]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 7853AllylamineHCID 516892Sodium BicarbonateHCID 18326549HCID 18326549、化合物

生成物 1

HCID 18326466HCID 18326466、化合物収率 56.9%

実験手順

189 mg (0.71 mmol) of 4-allylamino-2-chloro-7-propylthieno[3,2-d]pyrimidine and 644 mg (11.3 mmol) of allylamine were heated in a sealed tube at 140° C. for 16 hours. After completion of the reaction, the reaction mixture was allowed to resume room temperature, followed by adding a saturated aqueous sodium hydrogen carbonate solution thereto and extraction with ethyl acetate (50 ml×2). After the organic layer was washed with brine and dried over anhydrous sodium sulfate, the solvent was distilled off. The residue was purified by silica gel chromatography (eluent: ethyl acetate-hexane=1/4) to give 116 mg (yield: 56.9%) of the title compound.

後処理

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

出典と根拠

ORDレコード
ord-f2b1823152bd4da3a443804d28a843a7
出典データセット
uspto-grants-2002_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06339089B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート