N-bromobutanimide → HCID 66967418, 화합물

HRID 926238노트

반응식

HRID 926238 반응식
Br[CH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([Cl:9])[C:4]=1[O:10][CH3:11].ClC1C=CC(C)=C(OC)C=1.C1C(=O)[N:26](Br)[C:24](=O)C1>C(Cl)(Cl)Cl.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1>[Cl:9][C:5]1[C:4]([O:10][CH3:11])=[C:3]([CH2:2][CH2:24][NH2:26])[CH:8]=[CH:7][CH:6]=1

참가 물질

6

반응물 3

HCID 67184N-bromobutanimideHCID 2928585-Chloro-2-methylanisoleHCID 19390097HCID 19390097, 화합물

생성물 1

HCID 66967418HCID 66967418, 화합물

시약·촉매·용매 2

HCID 7187Benzoyl Peroxide촉매HCID 6212Chloroform용매

실험 절차

1-(bromomethyl)-3-chloro-2-methoxybenzene. A mixture of 4-chloro-2-methoxy-1-methylbenzene (26.5 g, 169 mmol), NBS (33.1 g, 186 mmol) and benzoyl peroxide (200 mg, 0.826 mmol) in CHCl3 was heated to reflux for 24 h. The reaction was allowed to cool to RT and then concentrated in vacuo. The residue was stirred with petroleum ether and the resulting suspension was filtered off and the filtrate was concentrated in vacuo to give the title compound (30.9 g) as brown oil, which was used as it is in the next step. UPLC (2 min) rt 1.708 min.

후처리

  1. temperaturewas heated
  2. temperatureto reflux for 24 h
  3. concentrationconcentrated in vacuo
  4. filtrationthe resulting suspension was filtered off
  5. concentrationthe filtrate was concentrated in vacuo

출처 및 근거

ORD 기록
ord-5704c7ec77fe40f696e68774708bafdc
출처 데이터셋
uspto-grants-2016_03
특허 번호
US09284331B2

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