Water → HCID 17963940、化合物

HRID 1375030ノート

反応式

HRID 1375030 の反応式
[O:1]1[CH2:6][CH2:5][NH:4][C:3]2[N:7]=[CH:8][CH:9]=[CH:10][C:2]1=2.[H-].[Na+].Cl[CH2:14][CH:15]1[O:19][CH2:18][CH2:17][O:16]1.O>CN(C)C=O.C(OCC)(=O)C>[O:16]1[CH2:17][CH2:18][O:19][CH:15]1[CH2:14][N:4]1[CH2:5][CH2:6][O:1][C:2]2[CH:10]=[CH:9][CH:8]=[N:7][C:3]1=2

参加物

7

反応物 4

HCID 962WaterHCID 24758Sodium hydrideHCID 757272-(Chloromethyl)-1,3-dioxolaneHCID 131965383,4-Dihydro-2H-pyrido(3,2-b)(1,4)oxazine

生成物 1

HCID 17963940HCID 17963940、化合物収率 42.9%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒2 回HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 3,4-dihydro-2H-pyrido[3,2-b]-1,4-oxazine (0.4 g) in N,N-dimethylformamide (5 ml) was added sodium hydride (60% oil suspension; 0.24 g) in portions. After a few minutes, a solution of 2-chloromethyl-1,3-dioxolane (0.43 g) in N,N-dimethylformamide (2 ml) was added dropwise to the mixture. After stirring for 2 hours, the mixture was poured into a mixed solvent of water and ethyl acetate. The organic layer was separated, washed with water twice, dried over magnesium sulfate and concentrated under reduced pressure. The residue was purified by column chromatography on silica gel using a mixed solvent of ethyl acetate and hexane (1:1) as an eluent to give 3,4-dihydro-4-[(1,3-dioxolan-2-yl)methyl]-2H-pyrido[3,2-b]-1,4-oxazine (0.28 g) as an oil.

後処理

  1. waitAfter a few minutes
  2. customThe organic layer was separated
  3. washwashed with water twice
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by column chromatography on silica gel using a mixed solvent of ethyl acetate and hexane (1:1) as an eluent

出典と根拠

ORDレコード
ord-36b9c7b9d91f4203a3065d62132580c1
出典データセット
uspto-grants-2007_01
特許番号
US07166598B2

反応ノート

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