Sodium Hydroxide → HCID 85728081、化合物

HRID 361297ノート

反応式

HRID 361297 の反応式
[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]

参加物

6

反応物 3

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

生成物 1

HCID 85728081HCID 85728081、化合物収率 98.7%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-d8f72326ee744defb68714492fa82820
出典データセット
uspto-grants-1999_02
特許番号
US05866513

反応ノート

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