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Water → 2-(4-Dimethoxymethyl-2-methoxy-3-nitrophenoxy)ethylamine

HRID 1821436
ノート
印刷プレビュー

反応式

HRID 1821436 の反応式
[CH3:1][O:2][CH:3]([O:29][CH3:30])[C:4]1[CH:23]=[CH:22][C:7]([O:8][CH2:9][CH2:10]C23C=CC=CC2C(NC3=O)=O)=[C:6]([O:24][CH3:25])[C:5]=1[N+:26]([O-:28])=[O:27].O.[NH2:32]N.O>C(O)C>[CH3:1][O:2][CH:3]([O:29][CH3:30])[C:4]1[CH:23]=[CH:22][C:7]([O:8][CH2:9][CH2:10][NH2:32])=[C:6]([O:24][CH3:25])[C:5]=1[N+:26]([O-:28])=[O:27]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 24654Hydrazine hydrate (1:1)HCID 866282232-[2-(4-Dimethoxymethyl-2-methoxy-3-nitrophenoxy)ethyl]phtalimide

生成物 1

HCID 689994632-(4-Dimethoxymethyl-2-methoxy-3-nitrophenoxy)ethylamine収率 116.4%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 2-[2-(4-dimethoxymethyl-2-methoxy-3-nitrophenoxy)ethyl]phtalimide (0.05 g, 0.12 mmol) obtained in Step 2 in ethanol (1.0 mL) was added with hydrazine monohydrate (6.4 μL, 0.13 mmol) and heated under reflux for 3 hours. The reaction mixture was cooled to room temperature and added with water, followed by extracting with ethyl acetate. The organic layer was washed with saturated brine, dried over anhydrous magnesium sulfate and the solvent was evaporated under reduced pressure to obtain 2-(4-dimethoxymethyl-2-methoxy-3-nitrophenoxy)ethylamine (0.04 g, 100%).

後処理

  1. temperatureheated
  2. temperatureunder reflux for 3 hours
  3. extractionby extracting with ethyl acetate
  4. washThe organic layer was washed with saturated brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customthe solvent was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-d2b8d37206694ab4b14e60d9a32a8f4f
出典データセット
uspto-grants-2009_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07605272B2

反応ノート

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