Sodium Hydroxide → HCID 85728081, 화합물

HRID 361297노트

반응식

HRID 361297 반응식
[CH3:1][O:2][C:3]1[C:10]([O:11][CH3:12])=[C:9]([O:13][CH3:14])[CH:8]=[CH:7][C:4]=1[CH:5]=O.Cl.[CH3:16][NH:17][OH:18].[OH-].[Na+]>C(O)C.O>[CH3:16][N+:17]([O-:18])=[CH:5][C:4]1[CH:7]=[CH:8][C:9]([O:13][CH3:14])=[C:10]([O:11][CH3:12])[C:3]=1[O:2][CH3:1]

참가 물질

6

반응물 3

HCID 14798Sodium HydroxideHCID 750062,3,4-TrimethoxybenzaldehydeHCID 77906N-methylhydroxylamine hydrochloride

생성물 1

HCID 85728081HCID 85728081, 화합물수율 98.7%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

To a stirred suspension of 9.97 g (50.9 mmol) of 2,3,4-trimethoxybenzaldehyde and 4.43 g (53.1 mmol) of N-methylhydroxylamine hydrochloride in 100 mL of ethanol was added a solution of 2.05 g (51.3 mmol) of sodium hydroxide in 15 mL of water. The mixture was stirred at room temperature for 22 h and evaporated in vacuo to remove the bulk of the solvent. The residual solid was taken up in 150 mL of dichloromethane, washed with 50 mL of water and dried over MgSO4. Removal of the solvent afforded 11.31 g of N-methyl-C-(2,3,4-trimethoxyphenyl)nitrone as a white solid. 1H-NMR (CDCl3) d 3.85-3.95 (9H), 6.75 (d, 1H), 7.65 (s, 1H), 9.1 (d, 1H).

후처리

  1. customevaporated in vacuo
  2. customto remove the bulk of the solvent
  3. washwashed with 50 mL of water
  4. dry with materialdried over MgSO4
  5. customRemoval of the solvent

출처 및 근거

ORD 기록
ord-d8f72326ee744defb68714492fa82820
출처 데이터셋
uspto-grants-1999_02
특허 번호
US05866513

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