Water → HCID 18173786、化合物

HRID 2399880ノート

反応式

HRID 2399880 の反応式
Cl[CH2:2][CH2:3][O:4][C:5]1[CH:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][CH:6]=1.[N-:14]=[N+:15]=[N-:16].[Li+].O>CN(C=O)C>[N:14]([CH2:2][CH2:3][O:4][C:5]1[CH:10]=[CH:9][C:8]([N+:11]([O-:13])=[O:12])=[CH:7][CH:6]=1)=[N+:15]=[N-:16]

参加物

5

反応物 3

HCID 962WaterHCID 88163Lithium azideHCID 27645871-(2-Chloroethoxy)-4-nitrobenzene

生成物 1

HCID 18173786HCID 18173786、化合物収率 97%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of 1.12 g (5.55 mmol) of 4-nitro 2-chloroethyl ether (Example 212) and lithium azide (544 mg, 11.1 mmol) in 3 mL of DMF was heated at 60° C. in an oil bath overnight under nitrogen atmosphere. The reaction was poured into water and extracted with ethyl acetate. The organics were washed with water and brine and dried over anhydrous magnesium sulfate and concentrated to give 1.12 g (97%) of the product: 1H NMR (200 MHz, CDCl3) δ8.18 (d, 2H, J=9Hz), 6.96 (d, 2H, J=9Hz), 4.21 (t, 2H, J=5Hz), 3.63 (t, 2H, J=5Hz).

後処理

  1. extractionextracted with ethyl acetate
  2. washThe organics were washed with water and brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-e21c0ad2a5874e68ba920e261cbc5836
出典データセット
uspto-grants-1995_09
特許番号
US05451677

反応ノート

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