Water → HCID 178522022、化合物

HRID 1361013

反応式

HRID 1361013 の反応式
[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

参加物

6

反応物 5

HCID 962WaterHCID 6228DimethylformamideHCID 25517Ammonium Chloride2 回HCID 33557Sodium Azide2 回HCID 752441-Naphthalenecarboxamide

生成物 1

HCID 178522022HCID 178522022、化合物収率 84%

反応条件

温度
125 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ad7e8a19ac1b4ecbaef897dc545dbbd1
出典データセット
uspto-grants-2011_02
特許番号
US07879893B2

関連ノート

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