Hydrochloric Acid → HCID 178419015、化合物

HRID 635127

反応式

HRID 635127 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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

4.99 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 were heated at 120° C. for 8 h in a 250 ml round-bottom flask fitted with a reflux condenser. After cooling to room temperature, 100 ml of water were added, and, in an ice bath, dilute hydrochloric acid was added until no more precipitate formed. The mixture was filtered with suction, and the precipitate was washed with water and dried. Recrystallization from ethanol/water produced 4.4 g of colorless crystals.

後処理

  1. customfitted with a reflux condenser
  2. customformed
  3. filtrationThe mixture was filtered with suction
  4. washthe precipitate was washed with water
  5. customdried
  6. customRecrystallization from ethanol/water

出典と根拠

ORDレコード
ord-0561e6e8c8e64a3dac1e01782ec069c9
出典データセット
uspto-grants-2001_02
特許番号
US06187224B1

関連ノート

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