Sodium borohydride → HCID 11459077、化合物

HRID 505356ノート

反応式

HRID 505356 の反応式
[CH2:1]1[O:17][C:16]2[CH:15]=[CH:14][C:5]([CH:6]=[N:7][CH2:8][CH:9]([O:12][CH3:13])[O:10][CH3:11])=[CH:4][C:3]=2[O:2]1.[BH4-].[Na+]>CO>[CH2:1]1[O:17][C:16]2[CH:15]=[CH:14][C:5]([CH2:6][NH:7][CH2:8][CH:9]([O:12][CH3:13])[O:10][CH3:11])=[CH:4][C:3]=2[O:2]1

参加物

4

反応物 2

HCID 4311764Sodium borohydrideHCID 11149084(3,4-Methylenedioxybenzylidene)-(2,2-dimethoxyethyl)amine

生成物 1

HCID 11459077HCID 11459077、化合物収率 46%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Imine 11b (10.74 g, 0.045 mol) was dissolved in methanol (100 mL) and NaBH4 (2×3 g) was added over 1 h while stirring the reaction mixture at room temperature. The reaction was quenched with methanol and the reaction mixture was concentrated and then diluted with diethyl ether (400 mL). The precipitate formed was removed by filtration. The filtrate was washed with water (2×200 mL), brine (200 mL), dried (Na2SO4) and concentrated to provide a yellow liquid (4.90 g, 46%). 1H NMR (300 MHz CDCl3) 6.79-6.69 (m, 3H), 5.86 (s, 2H), 4.41 (t, J=5.4 Hz, 1H), 3.64 (s, 2H), 3.30 (s, 6H), 2.65 (d, J=5.4 Hz, 2H).

後処理

  1. customThe reaction was quenched with methanol
  2. concentrationthe reaction mixture was concentrated
  3. additiondiluted with diethyl ether (400 mL)
  4. customThe precipitate formed
  5. customwas removed by filtration
  6. washThe filtrate was washed with water (2×200 mL), brine (200 mL)
  7. dry with materialdried (Na2SO4)
  8. concentrationconcentrated

出典と根拠

ORDレコード
ord-7cc22bd851464e53a38f6dfe0727dd42
出典データセット
uspto-grants-2010_08
特許番号
US07781445B2

反応ノート

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