Lawesson's reagent → tert-butyl N-(1-carbamothioyl-1-methylethyl)carbamate

HRID 927358노트

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HRID 927358 반응식
[NH2:1][C:2](=O)[C:3]([NH:6][C:7](=[O:13])[O:8][C:9]([CH3:12])([CH3:11])[CH3:10])([CH3:5])[CH3:4].COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:24])=CC=1>C1(C)C=CC=CC=1>[NH2:1][C:2](=[S:24])[C:3]([NH:6][C:7](=[O:13])[O:8][C:9]([CH3:12])([CH3:11])[CH3:10])([CH3:5])[CH3:4]

참가 물질

4

반응물 2

HCID 87949Lawesson's reagentHCID 11287144tert-Butyl (1-amino-2-methyl-1-oxopropan-2-yl)carbamate

생성물 1

HCID 15186362tert-butyl N-(1-carbamothioyl-1-methylethyl)carbamate수율 109.9%

시약·촉매·용매 1

HCID 1140Toluene용매

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온도
90 °C

실험 절차

To a mixture of tert-butyl 1-amino-2-methyl-1-oxopropan-2-ylcarbamate (10 g, 49 mmol) in toluene (200 mL) was added Lawesson's reagent (CAN 19172-47-5, 10 g, 25 mmol). The suspension was heated to 90° C. and stirred for 6 h. After evaporation of solvents, the residue was purified by column chromatography (silica gel, 120 g) eluting with 30% ethyl acetate in petroleum ether to yield the title compound (6 g, 56%); MS: m/e 241.2 [M+Na]+.

후처리

  1. customAfter evaporation of solvents
  2. customthe residue was purified by column chromatography (silica gel, 120 g)
  3. washeluting with 30% ethyl acetate in petroleum ether

출처 및 근거

ORD 기록
ord-ca15e275fac745d5af73e09e15b6e530
출처 데이터셋
uspto-grants-2016_03
특허 번호
US09290451B2

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