Sodium cyanoborohydride → HCID 15524191、化合物

HRID 1106427ノート

反応式

HRID 1106427 の反応式
Cl.[Br:2][C:3]1[CH:12]=[C:11]([N+:13]([O-:15])=[O:14])[C:10]([NH2:16])=[C:9]2[C:4]=1[CH2:5][CH2:6]N[CH2:8]2.[C:17]([BH3-])#[N:18].[Na+]>CO.O>[Br:2][C:3]1[CH:12]=[C:11]([N+:13]([O-:15])=[O:14])[C:10]([NH2:16])=[C:9]2[C:4]=1[CH2:5][CH2:6][N:18]([CH2:17][CH2:5][C:4]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:3]=1)[CH2:8]2

参加物

4

反応物 2

HCID 5003444Sodium cyanoborohydrideHCID 21253084HCID 21253084、化合物

生成物 1

HCID 15524191HCID 15524191、化合物収率 190.3%

試薬・触媒・溶媒 1

HCID 22242641Methanol--water (1/1)溶媒

実験手順

A solution of the product from Example 5 (1 g, 3.24 mmol) and phenylacetylaldehyde (0.82 ml, 7 mmol) in 2:1 MeOH/H2O (50 mL) was treated with sodium cyanoborohydride (0.56 g, 9 mmol) portionwise under nitrogen and stirred for one hour. The reaction mixture was then cooled under an ice bath and precipitate filtered off. The solids were washed with hexane and oven dried to give the title compound (1.16 g, 95% yield) as an orange solid, mp=120-122° C.

後処理

  1. temperatureThe reaction mixture was then cooled under an ice bath
  2. filtrationprecipitate filtered off
  3. washThe solids were washed with hexane and oven
  4. customdried

出典と根拠

ORDレコード
ord-fafda061af9644329d72ed6486bfa0ed
出典データセット
uspto-grants-2000_05
特許番号
US06057313

反応ノート

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