N-bromobutanimide → HCID 66967418、化合物

HRID 926238ノート

反応式

HRID 926238 の反応式
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

参加物

6

反応物 3

HCID 67184N-bromobutanimideHCID 2928585-Chloro-2-methylanisoleHCID 19390097HCID 19390097、化合物

生成物 1

HCID 66967418HCID 66967418、化合物

試薬・触媒・溶媒 2

HCID 7187Benzoyl Peroxide触媒HCID 6212Chloroform溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-5704c7ec77fe40f696e68774708bafdc
出典データセット
uspto-grants-2016_03
特許番号
US09284331B2

反応ノート

読み込み中…