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Hydrochloric Acid → 1-(3-Bromophenyl)-1-(3,4-difluoro-5-methoxyphenyl)-4-fluoro-1H-isoindol-3-amine

HRID 1662199
ノート
印刷プレビュー

反応式

HRID 1662199 の反応式
[Mg].[Li+].[Cl-].CC(C[AlH]CC(C)C)C.Br[C:14]1[CH:15]=[C:16]([O:22][CH3:23])[C:17]([F:21])=[C:18]([F:20])[CH:19]=1.[Br:24][C:25]1[CH:26]=[C:27]([C:31]([C:39]2[CH:44]=[CH:43][CH:42]=[C:41]([F:45])[C:40]=2[C:46]#[N:47])=[N:32]S(C(C)(C)C)=O)[CH:28]=[CH:29][CH:30]=1.Cl>C1COCC1.CO>[Br:24][C:25]1[CH:26]=[C:27]([C:31]2([C:14]3[CH:15]=[C:16]([O:22][CH3:23])[C:17]([F:21])=[C:18]([F:20])[CH:19]=3)[C:39]3[C:40](=[C:41]([F:45])[CH:42]=[CH:43][CH:44]=3)[C:46]([NH2:47])=[N:32]2)[CH:28]=[CH:29][CH:30]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 6

HCID 313Hydrochloric AcidHCID 14487Diisobutylaluminum hydrideHCID 433294Lithium ChlorideHCID 27732885-Bromo-1,2-difluoro-3-methoxybenzeneHCID 5462224MagnesiumHCID 76821598N-((3-bromophenyl)(2-cyano-3-fluorophenyl)methylene)-2-methylpropane-2-sulfinamide

生成物 1

HCID 58579507
1-(3-Bromophenyl)-1-(3,4-difluoro-5-methoxyphenyl)-4-fluoro-1H-isoindol-3-amine
収率 14%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒2 回HCID 8028Tetrahydrofuran溶媒4 回

実験手順

Magnesium turnings (0.692 g, 28.47 mmol) were stirred under Ar(g) for 10 min and LiCl 0.5M in THF (28.5 mL, 14.24 mmol) was added followed by DIBAL-H 1M in THF (0.228 mL, 0.23 mmol). The mixture was stirred for 5 min and then 5-bromo-1,2-difluoro-3-methoxybenzene (2.54 g, 11.39 mmol) in 5 mL THF was added in one portion and stirred for 1 h. The mixture was added to N-((3-bromophenyl)(2-cyano-3-fluorophenyl)methylene)-2-methylpropane-2-sulfinamide (4.64 g, 11.39 mmol) in THF (20 mL) and stirred 1 h. MeOH (3 mL) was added and the mixture was treated with HCl in 2.0 MeOH (22.78 mL, 22.78 mmol) for 1 h. NaHCO3(sat) was added and the mixture was extracted with EtOAc. The organic phase was washed with brine, dried over MgSO4 and concentrated. The residue was purified by preparative HPLC to give 714 mg (14%) of the title product as a solid. MS (ES+) m/z 447, 449 [M+H]+.

後処理

  1. stirringstirred for 1 h
  2. stirringstirred 1 h
  3. extractionthe mixture was extracted with EtOAc
  4. washThe organic phase was washed with brine
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated
  7. customThe residue was purified by preparative HPLC

出典と根拠

ORDレコード
ord-803baa96284448e9ad392a5f92265029
出典データセット
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08030500B2

反応ノート

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