Water → HCID 66695588、化合物

HRID 330817

反応式

HRID 330817 の反応式
[I:1][C:2]1[CH:9]=[CH:8][C:5]([CH:6]=O)=[CH:4][CH:3]=1.[NH2:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][N:12]=1.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+].O>C1COCC1>[I:1][C:2]1[CH:9]=[CH:8][C:5]([CH2:6][NH:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][N:12]=2)=[CH:4][CH:3]=1

参加物

6

反応物 4

HCID 962WaterHCID 104392-AminopyridineHCID 966574-IodobenzaldehydeHCID 5049666Sodium triacetoxyborohydride

生成物 1

HCID 66695588HCID 66695588、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
50 °C

実験手順

2.00 g (8.62 mmol) 4-iodo-benzaldehyde are added to 0.811 g (8.62 mmol) 2-amino-pyridine in 20 mL THF and the mixture is stirred for 1 h at 50° C. After that time, 4.57 g (21.5 mmol) sodium triacetoxyborohydride are added and the mixture is stirred for 1 h at 50° C. Subsequently, water is added and the mixture is extracted with EtOAc. The organic layer is dried over magnesium sulphate and the solvent is removed in vacuo. The residue is purified by RP-HPLC to yield the desired product.

後処理

  1. stirringthe mixture is stirred for 1 h at 50° C
  2. extractionthe mixture is extracted with EtOAc
  3. dry with materialThe organic layer is dried over magnesium sulphate
  4. customthe solvent is removed in vacuo
  5. customThe residue is purified by RP-HPLC

出典と根拠

ORDレコード
ord-ecc78df6dcc44bd7944d672c422118ab
出典データセット
uspto-grants-2014_11
特許番号
US08877754B2

関連ノート

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