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2-Fluoro-4-iodoaniline → (2-Dimethoxymethyl-3-fluoro-5-methoxy-6-nitro-phenyl)-(2-fluoro-4-iodo-phenyl)-amine

HRID 79044
ノート
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反応式

HRID 79044 の反応式
[F:1][C:2]1[CH:7]=[C:6]([I:8])[CH:5]=[CH:4][C:3]=1[NH2:9].[Li+].C[Si]([N-][Si](C)(C)C)(C)C.[CH3:20][O:21][CH:22]([O:36][CH3:37])[C:23]1[C:28](F)=[C:27]([N+:30]([O-:32])=[O:31])[C:26]([O:33][CH3:34])=[CH:25][C:24]=1[F:35]>C1COCC1>[CH3:37][O:36][CH:22]([O:21][CH3:20])[C:23]1[C:24]([F:35])=[CH:25][C:26]([O:33][CH3:34])=[C:27]([N+:30]([O-:32])=[O:31])[C:28]=1[NH:9][C:3]1[CH:4]=[CH:5][C:6]([I:8])=[CH:7][C:2]=1[F: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 3

HCID 1856942-Fluoro-4-iodoanilineHCID 2733832Lithium hexamethyldisilazaneHCID 58374324HCID 58374324、化合物

生成物 1

HCID 86656239(2-Dimethoxymethyl-3-fluoro-5-methoxy-6-nitro-phenyl)-(2-fluoro-4-iodo-phenyl)-amine収率 77%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

To a cold (−78° C.) solution of 2-fluoro-4-iodo-phenyl amine (2.97 g, 12.5 mmol) in THF (20 mL) was added LHMDS (24 mL, 1.0 M solution in hexanes 24 mmol) dropwise maintaining the temperature below −65° C. After stirring for 30 minutes a solution of 2-dimethoxymethyl-1,3-difluoro-5-methoxy-4-nitro-benzene (3.0 g, 11.4 mmol) in THF (20 mL) was added dropwise, the resultant mixture stirred cold (−78° C.) for 1 hour then allowed to warm to room temperature and stirred for 18 hours. The reaction was quenched by the addition of aqueous ammonium chloride and extracted twice with diethyl ether. The combined organic extracts were washed with water, dried (Na2SO4), filtered and concentrated in vacuo to give an orange solid. The crude orange solid was triturated in diethyl ether to give the title compound as a yellow solid (4.2 g, 77%). 1H NMR (CDCl3) 7.36 (1 H, dd, J=10.09, 1.93 Hz), 7.28-7.17 (2 H, m), 6.59 (1 H, t, J=8.62 Hz), 6.44 (1H, d, J=11.47 Hz), 5.49 (1 H, s), 3.88 (3 H, s), 3.39 (6 H, s).

後処理

  1. temperaturedropwise maintaining the temperature below −65° C
  2. additionwas added dropwise
  3. customThe reaction was quenched by the addition of aqueous ammonium chloride
  4. extractionextracted twice with diethyl ether
  5. washThe combined organic extracts were washed with water
  6. dry with materialdried (Na2SO4)
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo
  9. customto give an orange solid
  10. customThe crude orange solid was triturated in diethyl ether

出典と根拠

ORDレコード
ord-db06df38e0684729a8126a858fdb9c1e
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08841462B2

反応ノート

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