Hydrogen Peroxide → HCID 59339474, 화합물

HRID 1024369

반응식

HRID 1024369 반응식
[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

참가 물질

6

반응물 3

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

생성물 1

HCID 59339474HCID 59339474, 화합물수율 85%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-2a5a269aa70a42348b20b69165ffa7d2
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08722887B2

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