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

HRID 1740746ノート

反応式

HRID 1740746 の反応式
[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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-416c6c1fa3614fd2bd21670ad55b2a8c
出典データセット
uspto-grants-1999_10
特許番号
US05972935

反応ノート

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