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

HRID 2420252노트

반응식

HRID 2420252 반응식
[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

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 7187Benzoyl Peroxide촉매HCID 5943Carbon Tetrachloride용매2회

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-75fbd8abd1d048eeb44d46e67c54cb7e
출처 데이터셋
uspto-grants-1978_08
특허 번호
US04110345

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