Water → HCID 178419937、化合物

HRID 619350

反応式

HRID 619350 の反応式
[C:1]1([CH2:11][C:12]#[N:13])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1.[Cl-].[NH4+].[N-:16]=[N+:17]=[N-:18].[Na+].O>CN(C=O)C>[C:1]1([CH2:11][C:12]2[NH:18][N:17]=[N:16][N:13]=2)[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1

参加物

6

反応物 4

HCID 962WaterHCID 85961-NaphthaleneacetonitrileHCID 25517Ammonium ChlorideHCID 33557Sodium Azide

生成物 1

HCID 178419937HCID 178419937、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
125 °C

実験手順

A mixture of the above acetonitrile (5.40 g, 32 mmol), ammonium chloride (2.59 g, 48 mmol) and sodium azide (3.15 g, 48 mmol) in N,N'-dimethylformamide (100 ml) was stirred at 125° C. for 16 hours. After cooling the mixture was poured into water (300 ml) and extracted with ethyl acetate (2×150 ml) The combined organic phases were washed with water (100 ml) and evaporated in vacuo. The residue was crystallised from diethyl ether (20 ml), filtered off and washed with diethyl ether affording 1.86 g (27%) of the title compound as a solid.

後処理

  1. temperatureAfter cooling the mixture
  2. extractionextracted with ethyl acetate (2×150 ml) The combined organic phases
  3. washwere washed with water (100 ml)
  4. customevaporated in vacuo
  5. customThe residue was crystallised from diethyl ether (20 ml)
  6. filtrationfiltered off
  7. washwashed with diethyl ether affording 1.86 g (27%) of the title compound as a solid

出典と根拠

ORDレコード
ord-562e77285c9b4f8c81b0da662b8f4748
出典データセット
uspto-grants-1999_09
特許番号
US05958957

関連ノート

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