Bromotrimethylsilane → 6-(bromomethyl)-4-(3-methoxypropyl)-2H-benzo[b][1,4]oxazin-3(4H)-one

HRID 2246939노트

반응식

HRID 2246939 반응식
O[CH2:2][C:3]1[CH:4]=[CH:5][C:6]2[O:11][CH2:10][C:9](=[O:12])[N:8]([CH2:13][CH2:14][CH2:15][O:16][CH3:17])[C:7]=2[CH:18]=1.[Br:19][Si](C)(C)C>C(Cl)(Cl)Cl>[Br:19][CH2:2][C:3]1[CH:4]=[CH:5][C:6]2[O:11][CH2:10][C:9](=[O:12])[N:8]([CH2:13][CH2:14][CH2:15][O:16][CH3:17])[C:7]=2[CH:18]=1

참가 물질

4

반응물 2

HCID 76113BromotrimethylsilaneHCID 534011966-Hydroxymethyl-4-(3-methoxypropyl)-4H-benzo[1,4]oxazin-3-one

생성물 1

HCID 468352246-(bromomethyl)-4-(3-methoxypropyl)-2H-benzo[b][1,4]oxazin-3(4H)-one

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

To a solution of 74.0 g of 6-hydroxymethyl-4-(3-methoxy-propyl)-4H-benzo[1,4]oxazin-3-one (from example 1 g) in 600 ml of chloroform are added 58 ml of bromotrimethylsilane at room temperature. The reaction mixture is stirred for 30 minutes and concentrated under reduced pressure. The residue is purified by flash chromatography (SiO2 60 F) to afford the title compound as an off white solid. Rf=0.46 (EtOAc-heptane 1:1); Rt=4.03.

후처리

  1. customat room temperature
  2. concentrationconcentrated under reduced pressure
  3. customThe residue is purified by flash chromatography (SiO2 60 F)

출처 및 근거

ORD 기록
ord-b65de117807541049b7146a8232489c4
출처 데이터셋
uspto-grants-2010_03
특허 번호
US07687495B2

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