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Hydrochloric Acid → 5-(3-Amino-1-(3-bromophenyl)-4-fluoro-1H-isoindol-1-yl)-2-methoxy-3-methylbenzonitrile

HRID 1662218
ノート
印刷プレビュー

反応式

HRID 1662218 の反応式
[Mg].[Li+].[Cl-].CC(C[AlH]CC(C)C)C.Br[C:14]1[CH:15]=[C:16]([CH3:24])[C:17]([O:22][CH3:23])=[C:18]([CH:21]=1)[C:19]#[N:20].[Br:25][C:26]1[CH:27]=[C:28]([C:32]([C:40]2[CH:45]=[CH:44][CH:43]=[C:42]([F:46])[C:41]=2[C:47]#[N:48])=[N:33]S(C(C)(C)C)=O)[CH:29]=[CH:30][CH:31]=1.Cl>C1COCC1.CO>[NH2:48][C:47]1[C:41]2[C:40](=[CH:45][CH:44]=[CH:43][C:42]=2[F:46])[C:32]([C:14]2[CH:15]=[C:16]([CH3:24])[C:17]([O:22][CH3:23])=[C:18]([CH:21]=2)[C:19]#[N:20])([C:28]2[CH:29]=[CH:30][CH:31]=[C:26]([Br:25])[CH:27]=2)[N:33]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

10

反応物 6

HCID 313Hydrochloric AcidHCID 14487Diisobutylaluminum hydrideHCID 433294Lithium ChlorideHCID 5462224MagnesiumHCID 459232975-Bromo-2-methoxy-3-methylbenzonitrileHCID 76821598N-((3-bromophenyl)(2-cyano-3-fluorophenyl)methylene)-2-methylpropane-2-sulfinamide

生成物 1

HCID 58579494
5-(3-Amino-1-(3-bromophenyl)-4-fluoro-1H-isoindol-1-yl)-2-methoxy-3-methylbenzonitrile
収率 32%

試薬・触媒・溶媒 3

HCID 8028Tetrahydrofuran触媒HCID 887Methanol溶媒2 回HCID 8028Tetrahydrofuran溶媒3 回

実験手順

Magnesium turnings (37.3 mg, 1.53 mmol) were stirred under Ar(g) for 10 min and LiCl 0.5M in THF (1.841 mL, 0.92 mmol) was added followed by DIBAL-H 1M in THF (6.14 μL, 6.14 μmol). The mixture was stirred for 5 min and 5-bromo-2-methoxy-3-methylbenzonitrile (194 mg, 0.86 mmol) in THF (1 mL) was added in one portion and stirring was continued for 2 h. The solution was transferred via canula to N-((3-bromophenyl)(2-cyano-3-fluorophenyl)methylene)-2-methylpropane-2-sulfinamide (250 mg, 0.61 mmol) in THF (3 mL) at rt and stirred o.n. MeOH (4 mL) was added and the mixture was treated with HCl in MeOH (1.473 mL, 1.84 mmol) o.n. The solvents were removed in vacuo, and the residue was partitioned between saturated aqueous sodium bicarbonate solution and ethyl acetate. The combined organic layers were dried (Na2SO4), filtered and concentrated in vacuo. Purification by silica gel chromatography using a gradient of 0 to 2.5% (3.5 M ammonia in methanol) in dichloromethane afforded 0.088 g (32% yield) of the title compound.

後処理

  1. stirringstirring
  2. waitwas continued for 2 h
  3. stirringstirred o.n
  4. customThe solvents were removed in vacuo
  5. customthe residue was partitioned between saturated aqueous sodium bicarbonate solution and ethyl acetate
  6. dry with materialThe combined organic layers were dried (Na2SO4)
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo
  9. customPurification by silica gel chromatography

出典と根拠

ORDレコード
ord-b5b7e626cdd94c479392660a9367ecc3
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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