Methylamine → HCID 178482404, 화합물

HRID 33411노트

반응식

HRID 33411 반응식
Cl[C:2]1[CH:3]2[C:10]([I:11])=[CH:9][N:8]([CH:12]([CH3:14])[CH3:13])[CH:4]2[N:5]=[CH:6][N:7]=1.[CH3:15][NH2:16]>C1COCC1>[I:11][C:10]1[CH:3]2[CH:4]([N:5]=[CH:6][N:7]=[C:2]2[NH:16][CH3:15])[N:8]([CH:12]([CH3:14])[CH3:13])[CH:9]=1

참가 물질

4

반응물 2

HCID 6329MethylamineHCID 597965304-Chloro-7,7a-dihydro-5-iodo-7-isopropyl-4aH-pyrrolo[2,3-d]pyrimidine

생성물 1

HCID 178482404HCID 178482404, 화합물수율 85%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

4-Chloro-7,7a-dihydro-5-iodo-7-isopropyl-4aH-pyrrolo[2,3-d]pyrimidine (0.3 g, 0.93 mmol) from above was placed within a 15 ml pressure tube. 2 M methylamine in THF (15 ml) was added, and the reaction was left to stir overnight. The volatiles were removed in vacuo, and the residue was dissolved in methanol, 5 ml silica gel were added, and the volatiles were removed in vacuo. The adhered product was purified by silica gel chromatography (ethyl acetate:hexanes), and the requisite fractions were pooled and evaporated in vacuo to yield the desired product (0.25 g, 85% yield). 1H NMR (399.6 MHz, CDCl3) δ 1.43 (6H, d, J=6.8 Hz), 3.13 (3H, d, J=4.8 Hz), 5.0 (1H, sp, J=6.8 Hz), 7.02 (1H, s), 8.35 (1H, s).

후처리

  1. waitthe reaction was left
  2. customThe volatiles were removed in vacuo
  3. dissolutionthe residue was dissolved in methanol
  4. addition5 ml silica gel were added
  5. customthe volatiles were removed in vacuo
  6. customThe adhered product was purified by silica gel chromatography (ethyl acetate:hexanes)
  7. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-c8ab6941816542d796434313a961eab1
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07429596B2

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