Sodium Iodide → HCID 11514810、化合物

HRID 1801488ノート

反応式

HRID 1801488 の反応式
[NH2:1][C:2]1[CH:9]=[C:8]([O:10][CH2:11][CH2:12][CH2:13]Cl)[C:7]([O:15][CH3:16])=[CH:6][C:3]=1[C:4]#[N:5].[NH:17]1[CH2:22][CH2:21][O:20][CH2:19][CH2:18]1.[I-].[Na+]>>[NH2:1][C:2]1[CH:9]=[C:8]([O:10][CH2:11][CH2:12][CH2:13][N:17]2[CH2:22][CH2:21][O:20][CH2:19][CH2:18]2)[C:7]([O:15][CH3:16])=[CH:6][C:3]=1[C:4]#[N:5]

参加物

4

実験手順

A mixture of 2-amino-4-chloropropoxy-5-methoxy-benzonitrile (1.000 g, 4.12 mmol), morpholine (1.0 mL) and catalytic amount of sodium iodide were added into a round bottom flask. The solution was stirred and heated under reflux for 2 h. After reaction, extracted the solution with dichloromethane and water, and then combined the organic phases. After evaporating most of the solvent, equivalent amount of hydrochloric acid ether was added into the solution, and filtered to yield 1.100 g of white solid product with a recovery rate of 91%.

後処理

  1. additionwere added into a round bottom flask
  2. temperatureheated
  3. temperatureunder reflux for 2 h
  4. customAfter reaction
  5. extractionextracted the solution with dichloromethane and water
  6. customAfter evaporating most of the solvent, equivalent amount of hydrochloric acid ether
  7. additionwas added into the solution
  8. filtrationfiltered

出典と根拠

ORDレコード
ord-ef633660b14c4061a6222317d1f19bf8
出典データセット
uspto-grants-2013_01
特許番号
US08349835B2

反応ノート

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