Potassium Carbonate → HCID 86684662, 화합물

HRID 926430노트

반응식

HRID 926430 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

HCID 86684662HCID 86684662, 화합물수율 89.1%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-90e6db68316d4dfa927c48f9c825242b
출처 데이터셋
uspto-grants-2016_03
특허 번호
US09285319B2

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