Potassium Carbonate → HCID 86684662、化合物

HRID 926430ノート

反応式

HRID 926430 の反応式
Br[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][C:8]#[CH:9].[S:10]1[CH:14]=[CH:13][CH:12]=[C:11]1[C:15]1[N:23]=[C:22]([NH2:24])[N:21]=[C:20]2[C:16]=1[NH:17][CH:18]=[N:19]2.C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[S:10]1[CH:14]=[CH:13][CH:12]=[C:11]1[C:15]1[N:23]=[C:22]([NH2:24])[N:21]=[C:20]2[C:16]=1[N:17]=[CH:18][N:19]2[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][C:8]#[CH:9]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 111061218-bromo-1-octyneHCID 178143546-(Thiophen-2-yl)-7H-purin-2-amine

生成物 1

HCID 86684662HCID 86684662、化合物収率 89.1%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

8-Bromo-1-octyne (2.0 g, 10.6 mmol) prepared in step 1) was added to a dehydrated dimethylformamide (25 mL) solution containing 6-(thien-2-yl)-2-amino purine (1.2 g, 5.5 mmol) and potassium carbonate (2.3 g, 16.5 mmol), followed by stirring at room temperature for 15 hours. The reaction solution was concentrated and was separated between ethyl acetate and water. The organic layer was washed with saturated brine, was dried over anhydrous sodium sulfate, and was purified by medium-pressure preparative column chromatography to yield 6-(thien-2-yl)-9-(7-octynyl)-2-amino purine (1.6 g, 4.9 mmol, 87%).

後処理

  1. concentrationThe reaction solution was concentrated
  2. customwas separated between ethyl acetate and water
  3. washThe organic layer was washed with saturated brine
  4. dry with materialwas dried over anhydrous sodium sulfate
  5. customwas purified by medium-pressure preparative column chromatography

出典と根拠

ORDレコード
ord-90e6db68316d4dfa927c48f9c825242b
出典データセット
uspto-grants-2016_03
特許番号
US09285319B2

反応ノート

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