Hydrochloric Acid → HCID 178516885、化合物

HRID 1704747ノート

反応式

HRID 1704747 の反応式
[O:1]=[C:2]1[C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=2[O:5][CH:4]=[C:3]1[O:12][CH2:13][C:14]#[N:15].[N-:16]=[N+:17]=[N-:18].[Na+].[Cl-].[NH4+].Cl>CN(C=O)C.O>[NH:16]1[C:14]([CH2:13][O:12][C:3]2[C:2](=[O:1])[C:7]3[CH:8]=[CH:9][CH:10]=[CH:11][C:6]=3[O:5][CH:4]=2)=[N:15][N:18]=[N:17]1

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 25517Ammonium ChlorideHCID 33557Sodium AzideHCID 22758704HCID 22758704、化合物

生成物 1

HCID 178516885HCID 178516885、化合物収率 60%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
125 °C

実験手順

A mixture of [(4-oxo-4H-1-benzopyran-3-yl)oxy]acetonitrile (2.0 g, 0.01 mole), sodium azide (0.715 g, 0.011 mole) and ammonium chloride (0.56 g, 0.012 mole) in DMF (10 ml) is heated at 125° C. for 7 hrs. under nitrogen. The reaction is cooled overnight and then poured into excess cold water. The aqueous is acidified with 5N hydrochloric acid and the insoluble product is filtered, washed with fresh water and sucked dry. Recrystallization from absolute ethanol gives beige colored crystals (1.45 g, 60%), mp 194°-196° C.

後処理

  1. temperatureThe reaction is cooled overnight
  2. filtrationthe insoluble product is filtered
  3. washwashed with fresh water
  4. customsucked dry
  5. customRecrystallization from absolute ethanol

出典と根拠

ORDレコード
ord-75ec6efd058a426cadf5e032e2c887db
出典データセット
uspto-grants-1978_11
特許番号
US04127669

反応ノート

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