反応 #2286321

反応方程式

(3,5-dibromo-4-bromomethyl-phenyl)-methanol

(3,5-Dibromo-4-bromomethyl-phenyl)-methanol

6-(4-bromomethyl-2,6-dichloro-benzyl)-4-isopropyl-pyridazin-3-one

6-(4-Bromomethyl-2,6-dichloro-benzyl)-4-isopropyl-pyridazin-3-one

→

acetonitrile

収率 78.0%

(2,6-Dibromo-4-hydroxymethyl-phenyl)-acetonitrile

収率 78.0%

反応条件

後処理

1. 1
   その他This compound was prepared by a similar method to
2. 2
   その他The product was purified by flash chromatography
3. 3
   洗浄eluted with a gradient of 3:1 to 1:1 hexanes
4. 4
   その他The desired fractions were collected
5. 5
   濃縮concentrated under vacuum
6. 6
   その他to afford a solid which
7. 7
   その他was dried under high vacuum

実験手順

This compound was prepared by a similar method to that described in Example 14, Step 5 except that (3,5-dibromo-4-bromomethyl-phenyl)-methanol (58) was used in place 6-(4-bromomethyl-2,6-dichloro-benzyl)-4-isopropyl-pyridazin-3-one (54). The product was purified by flash chromatography using silica gel eluted with a gradient of 3:1 to 1:1 hexanes:ethyl acetate. The desired fractions were collected and concentrated under vacuum to afford a solid which was dried under high vacuum to afford 2,6-dibromo-4-hydroxymethyl-phenyl)-acetonitrile (59) (78%) as a yellow solid; EI(+)-HRMS m/z calcd for C9H7Br2NO (M 302.8894, found 302.8881. MW=304.9702, Exact Mass=302.8894

出典