Lawesson's reagent → HCID 86671704, 화합물

HRID 1748962노트

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HRID 1748962 반응식
[CH:1]1[C:13]2[CH2:12][C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[CH:3][C:2]=1[NH:14][C:15](=O)[CH:16]([CH3:18])[CH3:17].COC1C=CC(P2(=S)SP(=S)(C3C=CC(OC)=CC=3)[S:29]2)=CC=1>C1(C)C=CC=CC=1>[CH:1]1[C:13]2[CH2:12][C:11]3[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=3)[C:5]=2[CH:4]=[CH:3][C:2]=1[NH:14][C:15](=[S:29])[CH:16]([CH3:18])[CH3:17]

참가 물질

4

반응물 2

HCID 87949Lawesson's reagentHCID 148890Propionamide, N-(2-fluoren-yl)-2-methyl-

생성물 1

HCID 86671704HCID 86671704, 화합물수율 196.3%

시약·촉매·용매 1

HCID 1140Toluene용매

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온도
130 °C

실험 절차

In a 500 mL three-neck flask were put 20 g (80 mmol) of N-(9H-fluoren-2-yl)isobutyramide, 16 g (40 mmol) of 2,4-bis(4-methoxyphenyl)-1,3-dithia-2,4-diphosphetane-2,4-disulfide (Lawesson's reagent), and 150 mL of toluene, and the mixture was heated and refluxed at 130° C. for 4 hours. After that, the precipitated solid was washed with toluene and subjected to suction filtration to give 21 g of a yellow solid of N-(9H-fluoren-2-yl)isobutyrthioamide in a yield of 100%. The synthesis scheme of Step 2 is shown in (c-2) below.

후처리

  1. customIn a 500 mL three-neck flask were put
  2. washAfter that, the precipitated solid was washed with toluene
  3. filtrationsubjected to suction filtration

출처 및 근거

ORD 기록
ord-ad2eb7eaae9b4d70926e462687d2aadc
출처 데이터셋
uspto-grants-2015_10
특허 번호
US09155158B2

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