反応式
[CH3:1][C:2]1[N:7]=[CH:6][C:5]([CH2:8]O)=[CH:4][N:3]=1.C1(C)C=CC=CC=1.C1C=CC(OP(OC2C=CC=CC=2)([N:26]=[N+:27]=[N-:28])=O)=CC=1.N12CCCN=C1CCCCC2>O.C(Cl)Cl>[N:26]([CH2:8][C:5]1[CH:4]=[N:3][C:2]([CH3:1])=[N:7][CH:6]=1)=[N+:27]=[N-:28]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, 300 mmol) and methylene chloride (40 mL, 600 mmol) 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 for 2 h at 0° C. After being further stirred at rt for 16 h, the reaction mixture was diluted with water (50 mL) and DCM (50 mL). The organic layer was separated and washed with brine, dried (Mg2SO4), filtered, and concentration. The residue was purified by column to give the product as 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 column
出典と根拠
- ORDレコード
- ord-dc6dc165eeaa4449bbfc8b23cb514a24
- 出典データセット
- uspto-grants-2015_09
- 特許番号
- US09133122B2
関連ノート
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