Hydrochloric Acid → 1-Azido-2-chlorobenzene

HRID 2267125ノート

反応式

HRID 2267125 の反応式
Cl.[Cl:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[NH:9][NH2:10].Cl.[N:12]([O-])=O.[Na+]>C(OCC)C.O>[N:9]([C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][C:3]=1[Cl:2])=[N+:10]=[N-:12]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 4432872-Chlorophenylhydrazine hydrochlorideHCID 23668193Sodium Nitrite

生成物 1

HCID 114124881-Azido-2-chlorobenzene収率 59%

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 3283Diethyl Ether溶媒

反応条件

温度
0 °C

実験手順

2-Chlorophenylhydrazine hydrochloride (1.0 g) suspended in 6.0 ml of diethyl ether was dropped into 5 ml of concentrated hydrochloric acid cooled at 0° C. After the reaction solution was stirred for 10 minutes, 462 mg of sodium nitrite dissolved in 2.0 ml of water was dropped into the reaction solution and the mixture was stirred for 2 hours together with raising the temperature up to room temperature. Water was added to the reaction solution, the mixture was extracted with ethyl acetate and the ethyl acetate layer washed with a saturated aqueous saline solution and dried over sodium sulfate. The solvent was evaporated in vacuo to give 506 mg of the title compound as a red oily crude product.

後処理

  1. additionwas dropped into the reaction solution
  2. stirringthe mixture was stirred for 2 hours together
  3. temperaturewith raising the temperature up to room temperature
  4. extractionthe mixture was extracted with ethyl acetate
  5. washthe ethyl acetate layer washed with a saturated aqueous saline solution
  6. dry with materialdried over sodium sulfate
  7. customThe solvent was evaporated in vacuo

出典と根拠

ORDレコード
ord-b37e6e88d3cf497781369017a98275b6
出典データセット
uspto-grants-2010_12
特許番号
US07858800B2

反応ノート

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