Hydrochloric Acid → HCID 178418369, 화합물

HRID 1901

반응식

HRID 1901 반응식
CN(C)C=O.[C:6](#[N:13])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.[N-:14]=[N+:15]=[N-:16].[Na+].Cl>[Cl-].[Zn+2].[Cl-].O>[C:7]1([C:6]2[NH:16][N:15]=[N:14][N:13]=2)[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 6228DimethylformamideHCID 7505BenzonitrileHCID 33557Sodium Azide

생성물 1

HCID 178418369HCID 178418369, 화합물수율 90.1%

시약·촉매·용매 2

HCID 3007855Zincchloride촉매2회HCID 962Water용매

실험 절차

Zinc chloride (3.3 g, 24.3 mmol, 0.5 eq) was added to 15 mL of N,N-dimethylformamide in small portions while maintaining the temperature below 60° C. The suspension of zinc chloride was cooled to room temperature and treated with 5.0 g of benzonitrile (48.5 mmol, 1.0 eq) followed by 3.2 g of sodium azide (48.5 mmol, 1.0 eq). The heterogeneous mixture was heated at 115° C. with agitation for 18 hours. The mixture was cooled to room temperature, water (30 mL) was added and the mixture acidified by the addition of 5.1 mL of concentrated hydrochloric acid. The mixture was cooled to 0° C. and aged for one hour, then filtered and the filter cake washed with 15 mL of cold 0.1N HCl then dried at 60° C. under vacuum to afford 6.38 g (43.7 mmol, 90%) of the product.

후처리

  1. temperaturewhile maintaining the temperature below 60° C
  2. temperatureThe heterogeneous mixture was heated at 115° C. with agitation for 18 hours
  3. temperatureThe mixture was cooled to room temperature
  4. temperatureThe mixture was cooled to 0° C. and aged for one hour
  5. filtrationfiltered
  6. washthe filter cake washed with 15 mL of cold 0.1N HCl
  7. customthen dried at 60° C. under vacuum

출처 및 근거

ORD 기록
ord-683f6b06ba0444c18452d135760784ee
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05726319

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