Water → HCID 17963940, 화합물

HRID 1375030

반응식

HRID 1375030 반응식
[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

참가 물질

7

반응물 4

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

생성물 1

HCID 17963940HCID 17963940, 화합물수율 42.9%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매2회HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-36b9c7b9d91f4203a3065d62132580c1
출처 데이터셋
uspto-grants-2007_01
특허 번호
US07166598B2

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