Sodium Azide → 4-(2-Azidoethoxy)benzaldehyde

HRID 2362817ノート

反応式

HRID 2362817 の反応式
CC1C=CC(S(O[CH2:12][CH2:13][O:14][C:15]2[CH:20]=[CH:19][C:18]([CH:21]=[O:22])=[CH:17][CH:16]=2)(=O)=O)=CC=1.[N-:23]=[N+:24]=[N-:25].[Na+]>CN(C=O)C>[N:23]([CH2:12][CH2:13][O:14][C:15]1[CH:20]=[CH:19][C:18]([CH:21]=[O:22])=[CH:17][CH:16]=1)=[N+:24]=[N-:25]

参加物

4

反応物 2

HCID 33557Sodium AzideHCID 37755262-(4-Formylphenoxy)ethyl 4-methylbenzenesulfonate

生成物 1

HCID 179225524-(2-Azidoethoxy)benzaldehyde

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of 5.0 g (15.61 mmol) of the compound from Example 35A and 2.03 g (31.22 mmol) of sodium azide in 100 ml of dry DMF is stirred at RT for 12 h. The reaction mixture is concentrated using a rotary evaporator, and the residue is suspended in about 20 ml of water. After three extractions with in each case 30 ml of diethyl ether, the combined organic phases are washed twice with in each case 10 ml of water and once with 10 ml of saturated sodium chloride solution. After drying over sodium sulphate, the solvent is removed on a rotary evaporator.

後処理

  1. concentrationThe reaction mixture is concentrated
  2. customa rotary evaporator
  3. extractionAfter three extractions with in each case 30 ml of diethyl ether
  4. washthe combined organic phases are washed twice with in each case 10 ml of water and once with 10 ml of saturated sodium chloride solution
  5. dry with materialAfter drying over sodium sulphate
  6. customthe solvent is removed on a rotary evaporator

出典と根拠

ORDレコード
ord-cf136ad2a50a4b0d98b6a5fdae7a35fd
出典データセット
uspto-grants-2014_04
特許番号
US08691850B2

反応ノート

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