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Water → HCID 86660229, 화합물

HRID 2042714
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HRID 2042714 반응식
[Br:1][C:2]1[C:7]([NH2:8])=[CH:6][N:5]=[CH:4][N:3]=1.CC(C)([O-])C.[Na+].I[CH2:16][CH2:17][CH2:18][CH3:19].O>CC(N(C)C)=O>[Br:1][C:2]1[C:7]([NH:8][CH2:16][CH2:17][CH2:18][CH3:19])=[CH:6][N:5]=[CH:4][N:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 10962Butyl iodideHCID 23676156Sodium t-butoxideHCID 457897744-Bromopyrimidin-5-amine

생성물 1

HCID 86660229HCID 86660229, 화합물수율 22.7%

시약·촉매·용매 1

HCID 31374Dimethylacetamide용매

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온도
60 °C

실험 절차

A mixture of 4-bromopyrimidin-5-amine (1 g, 5.75 mmol), sodium tert-butoxide (1.11 g, 11.5 mmol) and 1-iodobutane (1.11 g, 6.03 mmol) in DMA (15 mL) was heated at 60° C. for 15 hours. The mixture was poured into water and extracted with ethyl acetate. The acetate layer was washed with water, brine, dried with MgSO4, filtered, and concentrated under reduced pressure. The residue was purified by chromatography (hexanes-EtOAc 3:1) to afford 300 mg of the title compound. MS (ESI) m/z 230 (M+H)+.

후처리

  1. extractionextracted with ethyl acetate
  2. washThe acetate layer was washed with water, brine
  3. dry with materialdried with MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by chromatography (hexanes-EtOAc 3:1)

출처 및 근거

ORD 기록
ord-509645f6c45b4840ad0ef5bbfb32b402
출처 데이터셋
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08586596B2

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