Triethylamine → HCID 58515970、化合物

HRID 717832ノート

反応式

HRID 717832 の反応式
[Cl:1][C:2]1[N+:11]([O-])=[CH:10][C:9]([Cl:13])=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5].[CH2:14]([N:16](CC)CC)C.C[Si](C#N)(C)C>C(#N)C>[Cl:1][C:2]1[N:11]=[C:10]([C:14]#[N:16])[C:9]([Cl:13])=[CH:8][C:3]=1[C:4]([O:6][CH3:7])=[O:5]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 82115Trimethylsilyl cyanideHCID 58515933HCID 58515933、化合物

生成物 1

HCID 58515970HCID 58515970、化合物収率 84.2%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
70 °C

実験手順

Methyl 2,5-dichloronicotinate 1-oxide (16 g, 72 mmol) was dissolved in acetonitrile (200 mL) with triethylamine (15 mL, 110 mmol) and trimethylsilyl cyanide (24 mL, 180 mmol) was added. The mixture was heated to 70° C. for 30 minutes. Evaporation and purification on silica gel using ethyl acetate in hexanes (0-30%) gave the desired compound (14 g, 82%). LCMS calculated for C8H5Cl2N2O2 (M+H)+: m/z=231.0. found: 230.8.

後処理

  1. additionwas added
  2. customEvaporation and purification on silica gel

出典と根拠

ORDレコード
ord-618b9b8c05174c1da84a1c9fd6469148
出典データセット
uspto-grants-2015_11
特許番号
US09193721B2

反応ノート

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