Hydrochloric Acid → HCID 178419015, 화합물

HRID 356797

반응식

HRID 356797 반응식
[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]

참가 물질

8

반응물 5

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

생성물 1

HCID 178419015HCID 178419015, 화합물수율 70.7%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-31833a1e0ad14612875a81cff3bd5702
출처 데이터셋
uspto-grants-1998_11
특허 번호
US05840217

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