Hydrochloric Acid → HCID 178419015、化合物

HRID 356797

反応式

HRID 356797 の反応式
[C:1]([C:5]1[CH:12]=[CH:11][C:8]([C:9]#[N:10])=[CH:7][CH:6]=1)([CH3:4])([CH3:3])[CH3:2].[Cl-].[Li+].[N-:15]=[N+:16]=[N-:17].[Na+].[Br-].C([NH+](CC)CC)C.Cl>CN(C=O)C.O>[C:1]([C:5]1[CH:6]=[CH:7][C:8]([C:9]2[NH:17][N:16]=[N:15][N:10]=2)=[CH:11][CH:12]=1)([CH3:4])([CH3:2])[CH3:3]

参加物

8

反応物 5

HCID 313Hydrochloric AcidHCID 12493Triethylamine hydrobromideHCID 33557Sodium AzideHCID 778834-tert-ButylbenzonitrileHCID 433294Lithium Chloride

生成物 1

HCID 178419015HCID 178419015、化合物収率 70.7%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

In a 250 ml round-bottomed flask fitted with reflux condenser, 4.9 g of p-t-butylbenzonitrile, 3.82 g of lithium chloride and 5.85 g of sodium azide and 8.2 g of triethylammonium bromide in 100 ml of DMF are heated at 120° C. for 8 hours. After cooling to room temperature, 100 ml of water are added and the mixture is admixed in an ice bath with dilute hydrochloric acid until no further solid precipitates. The precipitate is filtered off with suction, washed with water and dried. Recrystallization from ethanol/water gives 4.4 g of colorless crystals.

後処理

  1. customIn a 250 ml round-bottomed flask fitted
  2. temperaturewith reflux condenser
  3. customprecipitates
  4. filtrationThe precipitate is filtered off with suction
  5. washwashed with water
  6. customdried
  7. customRecrystallization from ethanol/water

出典と根拠

ORDレコード
ord-31833a1e0ad14612875a81cff3bd5702
出典データセット
uspto-grants-1998_11
特許番号
US05840217

関連ノート

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