Lawesson's reagent → HCID 58155249, 화합물

HRID 1929476노트

반응식

HRID 1929476 반응식
COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:10])=CC=1.[NH2:23][C:24]1[CH:25]=[C:26]([C:30]2([CH3:37])[NH:35][C:34](=O)[CH2:33][O:32][CH2:31]2)[CH:27]=[CH:28][CH:29]=1>COCCOC>[NH2:23][C:24]1[CH:25]=[C:26]([C:30]2([CH3:37])[NH:35][C:34](=[S:10])[CH2:33][O:32][CH2:31]2)[CH:27]=[CH:28][CH:29]=1

참가 물질

4

반응물 2

HCID 87949Lawesson's reagentHCID 581552585-(3-Amino-phenyl)-5-methyl-morpholin-3-one

생성물 1

HCID 58155249HCID 58155249, 화합물

시약·촉매·용매 1

HCID 80711,2-Dimethoxyethane용매

반응 조건

온도
80 °C

실험 절차

Lawesson's reagent (0.69 g, 1.64 mmol, 1.3 eq.) was added in one portion to a suspension of 5-(3-amino-phenyl)-5-methyl-morpholin-3-one (0.26 g, 1.26 mmol) in 1,2-dimethoxyethane (10 ml); the reaction mixture was stirred at 80° C. for 18 hours. After complete conversion, the solvent was partially removed at reduced pressure and the dark orange oil diluted with dichloromethane (5 ml) before washing with 1 M HCl (2×5 ml). The aqueous phase was brought to pH 8 and extracted with dichloromethane (4×10 ml) to yield the (RS)-5-(3-amino-phenyl)-5-methyl-morpholine-3-thione as a yellow oil (0.16 g, 57% of theory). Mass (calculated) C11H14N2OS [222.31]; (found) [M+H]+=223.

후처리

  1. customAfter complete conversion, the solvent was partially removed at reduced pressure
  2. additionthe dark orange oil diluted with dichloromethane (5 ml)
  3. washbefore washing with 1 M HCl (2×5 ml)
  4. extractionextracted with dichloromethane (4×10 ml)

출처 및 근거

ORD 기록
ord-ad25a09ae5b04e6186d93c67e6285d02
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08188079B2

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