7-Fluoro-5-nitro-2,3-dihydrobenzo[b][1,4]dioxine → 7-Fluoro-2,3-dihydro-1,4-benzodioxin-5-amine

HRID 1476766ノート

反応式

HRID 1476766 の反応式
[F:1][C:2]1[CH:3]=[C:4]([N+:12]([O-])=O)[C:5]2[O:10][CH2:9][CH2:8][O:7][C:6]=2[CH:11]=1>CO.[Pd]>[F:1][C:2]1[CH:3]=[C:4]([NH2:12])[C:5]2[O:10][CH2:9][CH2:8][O:7][C:6]=2[CH:11]=1

参加物

4

反応物 1

HCID 688171507-Fluoro-5-nitro-2,3-dihydrobenzo[b][1,4]dioxine

生成物 1

HCID 666806007-Fluoro-2,3-dihydro-1,4-benzodioxin-5-amine

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

10% Pd/C (400 mg) was added to a solution of 7-fluoro-5-nitro-2,3-dihydrobenzo[b][1,4]dioxine (2.0 g, 10 mmol) in methanol (50 mL) and stirring was continued at 25° C. under H2 atmosphere for 3 h. The reaction mixture was filtered over celite bed and washed with methanol. The filtrate and the washings were concentrated under reduced pressure to afford 7-fluoro-2,3-dihydrobenzo[b][1,4]dioxin-5-amine (Int-52) as pale brown liquid. MS (ESI): m/z 170.1 (M+H).

後処理

  1. filtrationThe reaction mixture was filtered over celite bed
  2. washwashed with methanol
  3. concentrationThe filtrate and the washings were concentrated under reduced pressure

出典と根拠

ORDレコード
ord-3d933e5eb70c495192de08fb045150d6
出典データセット
uspto-grants-2016_08
特許番号
US09402833B2

反応ノート

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