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N-bromobutanimide → 2-Bromo-5-(3-chloro-2-fluoro-phenyl)-6-(4-chloro-2-methyl-phenyl)-1-isopropyl-5,6-dihydro-1H-pyrrolo[3,4-b]pyrrol-4-one

HRID 2204290
ノート
印刷プレビュー

反応式

HRID 2204290 の反応式
C1C(=O)N([Br:8])C(=O)C1.[Cl:9][C:10]1[C:11]([F:36])=[C:12]([N:16]2[C:23](=[O:24])[C:22]3[CH:21]=[CH:20][N:19]([CH:25]([CH3:27])[CH3:26])[C:18]=3[CH:17]2[C:28]2[CH:33]=[CH:32][C:31]([Cl:34])=[CH:30][C:29]=2[CH3:35])[CH:13]=[CH:14][CH:15]=1>C(Cl)(Cl)(Cl)Cl.CCOC(C)=O>[Br:8][C:20]1[N:19]([CH:25]([CH3:27])[CH3:26])[C:18]2[CH:17]([C:28]3[CH:33]=[CH:32][C:31]([Cl:34])=[CH:30][C:29]=3[CH3:35])[N:16]([C:12]3[CH:13]=[CH:14][CH:15]=[C:10]([Cl:9])[C:11]=3[F:36])[C:23](=[O:24])[C:22]=2[CH:21]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 67184N-bromobutanimideHCID 867030935-(3-chloro-2-fluoro-phenyl)-6-(4-chloro-2-methyl-phenyl)-1-isopropyl-5,6-dihydro-1H-pyrrolo[3,4-b]pyrrol-4-one

生成物 1

HCID 867030922-Bromo-5-(3-chloro-2-fluoro-phenyl)-6-(4-chloro-2-methyl-phenyl)-1-isopropyl-5,6-dihydro-1H-pyrrolo[3,4-b]pyrrol-4-one

試薬・触媒・溶媒 2

HCID 5943Carbon Tetrachloride溶媒HCID 8857
Ethyl Acetate
溶媒

実験手順

NBS (1.926 mmol) was added to a mixture of 5-(3-chloro-2-fluoro-phenyl)-6-(4-chloro-2-methyl-phenyl)-1-isopropyl-5,6-dihydro-1H-pyrrolo[3,4-b]pyrrol-4-one (Step A1) (1.965 mmol) in CCl4 (65 mL). After 1.5 h, the reaction mixture was diluted with EtOAc and successively washed with a saturated aqueous solution of NaHCO3, water and brine, dried (Na2SO4), filtered and concentrated. The residue was purified using a RediSep® silica gel column to afford the title compound as a white solid. tR: 5.69 min (HPLC 1); ESI-MS: tR=1.39 min, [M+H]+ 495/497/499 (LC-MS 1); TLC: Rf=0.12 (CH2Cl2).

後処理

  1. washsuccessively washed with a saturated aqueous solution of NaHCO3, water and brine
  2. dry with materialdried (Na2SO4)
  3. filtrationfiltered
  4. concentrationconcentrated
  5. customThe residue was purified

出典と根拠

ORDレコード
ord-4090b389d522457f9e416a188aba0b11
出典データセット
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09365576B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート