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2-Methoxyethanol → HCID 18332788, 화합물

HRID 2269147
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HRID 2269147 반응식
[NH2:1][C:2]1[N:10]=[CH:9][N:8]=[C:7]2[C:3]=1[N:4]=[CH:5][N:6]2[CH2:11][C:12]1[CH:17]=[CH:16][C:15]([F:18])=[CH:14][CH:13]=1.[CH3:19][O:20][CH2:21][CH2:22][OH:23]>[Na]>[NH2:1][C:2]1[N:10]=[C:9]([O:23][CH2:22][CH2:21][O:20][CH3:19])[N:8]=[C:7]2[C:3]=1[N:4]=[CH:5][N:6]2[CH2:11][C:12]1[CH:17]=[CH:16][C:15]([F:18])=[CH:14][CH:13]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 80192-MethoxyethanolHCID 114364636-Amino-9-(4-fluorobenzyl)purine

생성물 1

HCID 18332788HCID 18332788, 화합물수율 95%

시약·촉매·용매 1

HCID 5360545Sodium용매

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온도
20 °C

실험 절차

6-Amino-9-(4-fluorobenzyl)purine (100 mg, 0.36 mmol) was dissolved in 30 ml of sodium 2-mehoxyethoxide in 2-methoxyethanol and the solution was heated at 20° C. for 3 hours. The reaction mixture was concentrated in vacuo to dryness and to the residue was added water. The mixture was extracted with chloroform and the organic layer was washed with water, dried on sodium sulfate and concentrated in vacuo to dryness. The residue was purified with silica gel chromatography (2% methanol/chloroform) to give the subject compound (109 mg, yield 95%).

후처리

  1. concentrationThe reaction mixture was concentrated in vacuo to dryness and to the residue
  2. additionwas added water
  3. extractionThe mixture was extracted with chloroform
  4. washthe organic layer was washed with water
  5. customdried on sodium sulfate
  6. concentrationconcentrated in vacuo to dryness
  7. customThe residue was purified with silica gel chromatography (2% methanol/chloroform)

출처 및 근거

ORD 기록
ord-362e64275a76417da4b34e10cad399eb
출처 데이터셋
uspto-grants-2001_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06329381B1

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