1,3-Dibromopropane → 2H-1,4-Benzoxazine, 4-(3-bromopropyl)-3,4-dihydro-

HRID 901827ノート

反応式

HRID 901827 の反応式
[O:1]1[CH2:6][CH2:5][NH:4][C:3]2[CH:7]=[CH:8][CH:9]=[CH:10][C:2]1=2.[Br:11][CH2:12][CH2:13][CH2:14]Br.C(=O)([O-])[O-].[Na+].[Na+]>CN(C=O)C.C(OCC)(=O)C>[O:1]1[CH2:6][CH2:5][N:4]([CH2:14][CH2:13][CH2:12][Br:11])[C:3]2[CH:7]=[CH:8][CH:9]=[CH:10][C:2]1=2

参加物

6

反応物 3

HCID 80011,3-DibromopropaneHCID 10340Sodium CarbonateHCID 5850963,4-Dihydro-2H-1,4-benzoxazine

生成物 1

HCID 114708452H-1,4-Benzoxazine, 4-(3-bromopropyl)-3,4-dihydro-

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
70 °C

実験手順

A mixture of 3,4-dihydro-2H-benzo[b][1,4]oxazine (3.0 g, 1 eq, 22.2 mmol), 1,3-dibromopropane (22.5 ml, 10 eq, 222 mmol) and anhydrous sodium carbonate (7.05 g, 3 eq, 66.6 mmol) in dry DMF (200 ml) was heated at 70° C. for 16 h. The reaction mixture was diluted with ethyl acetate and washed with water and brine. The residue was chromatographed using ethyl acetate and hexane to yield the title compounds as liquid mass (2.6 g, 47%).

後処理

  1. washwashed with water and brine
  2. customThe residue was chromatographed

出典と根拠

ORDレコード
ord-538ea71e18814810a68e0e9c5a8608eb
出典データセット
uspto-grants-2008_04
特許番号
US07365064B2

反応ノート

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