反応式
[CH3:1][C:2]1[N:7]=[CH:6][C:5]([CH2:8]O)=[CH:4][N:3]=1.C1C=CC(OP(OC2C=CC=CC=2)([N:19]=[N+:20]=[N-:21])=O)=CC=1.N12CCCN=C1CCCCC2>C1(C)C=CC=CC=1.C(Cl)Cl.O>[N:19]([CH2:8][C:5]1[CH:4]=[N:3][C:2]([CH3:1])=[N:7][CH:6]=1)=[N+:20]=[N-:21]参加物
7
反応条件
- 温度
- 0 °C
実験手順
A solution of (2-methylpyrimidin-5-yl)methanol (0.82 g, 6.6 mmol) in toluene (30 mL) and methylene chloride (40 mL) at 0° C. was treated with diphenylphosphonic azide (2.8 mL, 13 mmol) followed by 1,8-diazabicyclo[5.4.0]undec-7-ene (2.0 mL, 13 mmol) and stirred at 0° C. for 2 h. After being further stirred at rt for 16 h, the reaction mixture was diluted with water (50 mL) and methylene chloride (50 mL). The organic layer was separated and washed with brine, dried (Mg2SO4), filtered, and concentration. The residue was purified by silica gel column to yield a colorless oil.
後処理
- stirringAfter being further stirred at rt for 16 h
- customThe organic layer was separated
- washwashed with brine
- dry with materialdried (Mg2SO4)
- filtrationfiltered
- concentrationconcentration
- customThe residue was purified by silica gel column
- customto yield a colorless oil
出典と根拠
- ORDレコード
- ord-3d3d0b07d9b84da49fe303d46f429500
- 出典データセット
- uspto-grants-2011_12
- 特許番号
- US08076345B2
関連ノート
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