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Sodium Methoxide → HCID 67428565, 화합물

HRID 1660754
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HRID 1660754 반응식
Br[C:2]1[N:3]=[C:4]([N:23]2[CH2:28][CH2:27][O:26][CH2:25][CH2:24]2)[S:5][C:6]=1[C:7]1[C:8]([CH3:22])=[N:9][N:10]2[C:15]([CH:16]([CH2:19][CH3:20])[CH2:17][CH3:18])=[CH:14][C:13]([CH3:21])=[N:12][C:11]=12.[CH3:29][O-:30].[Na+]>CO.[Cu]I>[CH2:17]([CH:16]([C:15]1[N:10]2[N:9]=[C:8]([CH3:22])[C:7]([C:6]3[S:5][C:4]([N:23]4[CH2:28][CH2:27][O:26][CH2:25][CH2:24]4)=[N:3][C:2]=3[O:30][CH3:29])=[C:11]2[N:12]=[C:13]([CH3:21])[CH:14]=1)[CH2:19][CH3:20])[CH3:18]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 10942334Sodium MethoxideHCID 67428983HCID 67428983, 화합물

생성물 1

HCID 67428565HCID 67428565, 화합물수율 13.8%

시약·촉매·용매 2

HCID 24350Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)촉매HCID 887Methanol용매

실험 절차

Stir a mixture of 3-(4-bromo-2-morpholin-4-yl-thiazol-5-yl)-7-(1-ethyl-propyl)-2,5-dimethyl-pyrazolo[1,5-a]pyrimidine (162 mg, 0.35 mmol), sodium methoxide (57 mg, 1.05 mmol) and copper(I) iodide (67 mg, 0.35 mmol) in methanol (3 mL) in a sealed 4-mL vial for 15 h at 120° C. Cool to room temperature, remove the solid by filtration, and concentrate the filtrate under vacuum. Purify the residue by flash chromatography, eluting with hexanes/THF (10/2). Recrystallize the material from methanol to give the title compound (20 mg). ES/MS m/z 416.0 (M+1)+.

후처리

  1. customremove the solid
  2. filtrationby filtration
  3. concentrationconcentrate the filtrate under vacuum
  4. customPurify the residue by flash chromatography
  5. washeluting with hexanes/THF (10/2)
  6. customRecrystallize the material from methanol

출처 및 근거

ORD 기록
ord-8c7023446dbc4642b27377b41b0e1a97
출처 데이터셋
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08030304B2

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