Triethylamine → HCID 58515970, 화합물

HRID 717832노트

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HRID 717832 반응식
[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]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 82115Trimethylsilyl cyanideHCID 58515933HCID 58515933, 화합물

생성물 1

HCID 58515970HCID 58515970, 화합물수율 84.2%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

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온도
70 °C

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-618b9b8c05174c1da84a1c9fd6469148
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09193721B2

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