Hydrogen Peroxide → HCID 59339474、化合物

HRID 1024369

反応式

HRID 1024369 の反応式
[NH2:1][CH2:2][C:3]1([CH2:9][NH2:10])[CH2:8][CH2:7][O:6][CH2:5][CH2:4]1.OO.[O-]Cl.[Na+]>O.CO>[CH2:9]1[C:3]2([CH2:8][CH2:7][O:6][CH2:5][CH2:4]2)[CH2:2][N:1]=[N:10]1

参加物

6

反応物 3

HCID 784Hydrogen PeroxideHCID 68738[4-(Aminomethyl)oxan-4-yl]methanamineHCID 23665760Sodium Hypochlorite

生成物 1

HCID 59339474HCID 59339474、化合物収率 85%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

C-(4-Aminomethyl-tetrahydro-pyran-4-yl)-methylamine (1.0 g) was taken up in a mixture of H2O (10 mL) and MeOH (2.5 mL), and cooled in an ice bath. Simultaneously, H2O2 (4.8 mL of a 30% solution, 6 equiv.) and NaClO (12.4 mL of a 10% solution, 2.4 equiv.) were added dropwise, the ice bath was removed, and the mixture was stirred overnight at room temperature. Extraction with DCM, drying over Na2SO4 and evaporation under reduced pressure yielded 380 mg of a clear, light-yellow liquid containing 85% of the anticipated product and 15% of the diamine starting material. This material was used in subsequent steps without further purification. 1H NMR (400 MHz, CDCl3) δ 1.49 (t, 4H), 3.65 (t, 4H), 4.28 (s, 4H).

後処理

  1. temperaturecooled in an ice bath
  2. customthe ice bath was removed
  3. extractionExtraction with DCM
  4. dry with materialdrying over Na2SO4 and evaporation under reduced pressure
  5. customyielded 380 mg of a clear, light-yellow liquid

出典と根拠

ORDレコード
ord-2a5a269aa70a42348b20b69165ffa7d2
出典データセット
uspto-grants-2014_05
特許番号
US08722887B2

関連ノート

読み込み中…