Acetaldehyde, 2,2-dimethoxy- → 3,4-Dihydro-6-(2,2-dimethoxyethyl)amino-4-(2-dimethylaminoethyl)-2H-1,4-benzoxazine

HRID 1740746노트

반응식

HRID 1740746 반응식
[NH2:1][C:2]1[CH:3]=[CH:4][C:5]2[O:10][CH2:9][CH2:8][N:7]([CH2:11][CH2:12][N:13]([CH3:15])[CH3:14])[C:6]=2[CH:16]=1.[CH3:17][O:18][CH:19]([O:22][CH3:23])[CH:20]=O>[Pd].C(O)C>[CH3:17][O:18][CH:19]([O:22][CH3:23])[CH2:20][NH:1][C:2]1[CH:3]=[CH:4][C:5]2[O:10][CH2:9][CH2:8][N:7]([CH2:11][CH2:12][N:13]([CH3:14])[CH3:15])[C:6]=2[CH:16]=1

참가 물질

5

반응물 2

HCID 162650Acetaldehyde, 2,2-dimethoxy-HCID 106805166-Amino-3,4-dihydro-4-(2-dimethylaminoethyl)-2H-1,4-benzoxazine

생성물 1

HCID 218330383,4-Dihydro-6-(2,2-dimethoxyethyl)amino-4-(2-dimethylaminoethyl)-2H-1,4-benzoxazine수율 77%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

실험 절차

6-Amino-3,4-dihydro-4-(2-dimethylaminoethyl)-2H-1,4-benzoxazine (D3, 1.78 g, 8.1 mmol) and dimethoxyacetaldehyde (40% in MTBE, 3.1 g) were hydrogenated over 10% palladium on carbon (0.5g) in ethanol (70 ml) for 24 h. The catalyst was filtered off, and the filtrate was evaporated to dryness. The residue was dissolved in ethyl acetate, washed with water and brine, dried (Na2SO4) and evaporated to give the title compound (1.92 g, 77%) as a brown oil.

후처리

  1. filtrationThe catalyst was filtered off
  2. customthe filtrate was evaporated to dryness
  3. dissolutionThe residue was dissolved in ethyl acetate
  4. washwashed with water and brine
  5. dry with materialdried (Na2SO4)
  6. customevaporated

출처 및 근거

ORD 기록
ord-416c6c1fa3614fd2bd21670ad55b2a8c
출처 데이터셋
uspto-grants-1999_10
특허 번호
US05972935

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