N-bromobutanimide → 5-(bromomethyl)-2,2-difluorobenzo[d][1,3]dioxole

HRID 2420252ノート

反応式

HRID 2420252 の反応式
[F:1][C:2]1([F:12])[O:6][C:5]2[CH:7]=[CH:8][C:9]([CH3:11])=[CH:10][C:4]=2[O:3]1.[Br:13]N1C(=O)CCC1=O>C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1.C(Cl)(Cl)(Cl)Cl>[F:12][C:2]1([F:1])[O:6][C:5]2[CH:7]=[CH:8][C:9]([CH2:11][Br:13])=[CH:10][C:4]=2[O:3]1

参加物

5

反応物 2

HCID 67184N-bromobutanimideHCID 138788692,2-Difluoro-5-methyl-2H-1,3-benzodioxole

生成物 1

HCID 203113835-(bromomethyl)-2,2-difluorobenzo[d][1,3]dioxole収率 96.6%

試薬・触媒・溶媒 2

HCID 7187Benzoyl Peroxide触媒HCID 5943Carbon Tetrachloride溶媒2 回

実験手順

A mixture of 2,2-difluoro-5-methyl-1,3-benzodioxole (29.0 g, 0.169 mole), N-bromosuccinimide (30.1 g, 0.169 mole), benzoyl peroxide (0.5 g) and carbon tetrachloride (50 ml) is refluxed for 2.5 hours. Carbon tetrachloride (50 ml) is then added to the hot reaction mixture and the solids are filtered off. The filtrate and washings are evaporated to yield 41.0 g of title product, a brown oil; nmr (CCl4) δ 4.38 (S, 2H), 6.8-7.4 (m, 3H). The product is used without further purification in the next step.

後処理

  1. temperatureis refluxed for 2.5 hours
  2. filtrationthe solids are filtered off
  3. customThe filtrate and washings are evaporated

出典と根拠

ORDレコード
ord-75fbd8abd1d048eeb44d46e67c54cb7e
出典データセット
uspto-grants-1978_08
特許番号
US04110345

反応ノート

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