Lawesson's reagent → N-[2-(3-cyanophenoxy)ethyl]-4-cyanobenzthioamide

HRID 747659노트

반응식

HRID 747659 반응식
[C:1]([C:3]1[CH:4]=[C:5]([CH:20]=[CH:21][CH:22]=1)[O:6][CH2:7][CH2:8][NH:9][C:10](=O)[C:11]1[CH:16]=[CH:15][C:14]([C:17]#[N:18])=[CH:13][CH:12]=1)#[N:2].COC1C=CC(P2(=S)SP(=S)(C3C=CC(OC)=CC=3)[S:32]2)=CC=1>C1(C)C=CC=CC=1>[C:1]([C:3]1[CH:4]=[C:5]([CH:20]=[CH:21][CH:22]=1)[O:6][CH2:7][CH2:8][NH:9][C:10](=[S:32])[C:11]1[CH:16]=[CH:15][C:14]([C:17]#[N:18])=[CH:13][CH:12]=1)#[N:2]

참가 물질

4

반응물 2

HCID 87949Lawesson's reagentHCID 11066232N-[2-(3-cyanophenoxy)ethyl]-4-cyanobenzamide

생성물 1

HCID 17788792N-[2-(3-cyanophenoxy)ethyl]-4-cyanobenzthioamide

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

1.46 g (5.00 mmol)) of N-[2-(3-cyanophenoxy)ethyl]-4-cyanobenzamide was dissolved in 50 ml of toluene. 3.03 g (7.5 mmol) of 2,4-bis(4-methoxyphenyl)-1,3-dithia-2,4-diphosphetane-2,4-disulfide was added to the solution, and the obtained mixture was heated under reflux for 4 hours. The precipitate was removed by the filtration, and the solvent was evaporated under reduced pressure. The residue was purified by the silica gel column chromatography, and the title compound was obtained.

후처리

  1. temperaturethe obtained mixture was heated
  2. temperatureunder reflux for 4 hours
  3. customThe precipitate was removed by the filtration
  4. customthe solvent was evaporated under reduced pressure
  5. customThe residue was purified by the silica gel column chromatography

출처 및 근거

ORD 기록
ord-1e97c0a040234ce3a4afe08aef55cf13
출처 데이터셋
uspto-grants-2008_07
특허 번호
US07396844B1

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