Water → HCID 178522022, 화합물

HRID 1361013

반응식

HRID 1361013 반응식
[C:1]1(C(N)=O)[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1.[N-:14]=[N+:15]=[N-:16].[Na+].[Cl-].[NH4+:19].O.[CH3:21][N:22](C)[CH:23]=[O:24]>>[NH:14]1[C:5]([C:10]2[CH:9]=[C:21]([NH:22][C:23]([C:3]3[CH:2]=[CH:1][C:10]4[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=4)[CH:4]=3)=[O:24])[CH:3]=[CH:2][CH:1]=2)=[N:19][N:16]=[N:15]1

참가 물질

6

반응물 5

HCID 962WaterHCID 6228DimethylformamideHCID 25517Ammonium Chloride2회HCID 33557Sodium Azide2회HCID 752441-Naphthalenecarboxamide

생성물 1

HCID 178522022HCID 178522022, 화합물수율 84%

반응 조건

온도
125 °C

실험 절차

The above naphthoic acid amide (10 g, 37 mmol) was dissolved in N,N-dimethylformamide (200 mL) and sodium azide (2.63 g, 40 mmol) and ammonium chloride (2.16 g, 40 mmol) were added and the mixture heated at 125° C. for 6 hours. Sodium azide (1.2 g) and ammonium chloride (0.98 g) were added and the mixture heated at 125° C. for 16 hours. After cooling, the mixture was poured into water (1.5 l) and stirred at room temperature for 30 minutes. The solid formed was filtered off, washed with water and dried in vacuo at 50° C. for 3 days affording 9.69 g (84%) of the title compound as a solid which could be further purified by treatment with ethanol at reflux temperature.

후처리

  1. temperaturethe mixture heated at 125° C. for 16 hours
  2. temperatureAfter cooling
  3. customThe solid formed
  4. filtrationwas filtered off
  5. washwashed with water
  6. customdried in vacuo at 50° C. for 3 days

출처 및 근거

ORD 기록
ord-ad7e8a19ac1b4ecbaef897dc545dbbd1
출처 데이터셋
uspto-grants-2011_02
특허 번호
US07879893B2

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