Methylamine → HCID 178482404、化合物

HRID 33411ノート

反応式

HRID 33411 の反応式
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

参加物

4

反応物 2

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

生成物 1

HCID 178482404HCID 178482404、化合物収率 85%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-c8ab6941816542d796434313a961eab1
出典データセット
uspto-grants-2008_09
特許番号
US07429596B2

反応ノート

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