Acetonitrile → 4-(2-Pyrimidinyl)-3-butynol
反応式
Br[C:2]1[N:7]=[CH:6][CH:5]=[CH:4][N:3]=1.[CH2:8]([OH:12])[CH2:9][C:10]#[CH:11].C1(NC2CCCCC2)CCCCC1.C(#N)C>[Cu]I.CCOCC>[N:3]1[CH:4]=[CH:5][CH:6]=[N:7][C:2]=1[C:11]#[C:10][CH2:9][CH2:8][OH:12]参加物
7
実験手順
A mixture of 2-bromopyrimidine (5.0 g), 3-butynol (2.20 g), dicyclohexylamine (6.87 g), copper (1) iodide (50 mg). BTPC (380 mg) and acetonitrile (50 ml) was stirred at room temperature under nitrogen for 16 h. Ether (150 ml) was added, the mixture filtered and the filtrate evaporated in vacuo. Purification of the residue by FCC eluting with ether and ether-methanol (1-3%) followed by System C (5:1) afforded the title compound as a pale yellow solid (4.29 g) m.p. 58°-64°, t.l.c. (System C, 99:1) Rf 0.08
後処理
- filtrationthe mixture filtered
- customthe filtrate evaporated in vacuo
- customPurification of the residue by FCC
- washeluting with ether and ether-methanol (1-3%)
出典と根拠
- ORDレコード
- ord-4c2d310dfa3b4836a05ff9595b7d5905
- 出典データセット
- uspto-grants-1991_02
- 特許番号
- US04996218
反応ノート
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