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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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2-Naphthalenecarboxamide → Naphthalene-2-carbothioamide

HRID 1107896
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HRID 1107896 반응식
[CH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][C:2]=1[C:11]([NH2:13])=O.COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:23])=CC=1>O1CCCC1>[CH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][C:2]=1[C:11](=[S:23])[NH2:13]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 752452-NaphthalenecarboxamideHCID 87949Lawesson's reagent

생성물 1

HCID 2800333Naphthalene-2-carbothioamide수율 83%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of the above amide (10.0 g, 58 mmol) in dry tetrahydrofuran (250 ml) was added [2,4-bis-(4-methoxyphenyl)-1,3-dithia-2,4-diphosphenate-2,4-disulfide] (Lawesson's reagent) (16.5 g, 41 mmol) and the resulting mixture was stirred at room temperature for 48 h. The volatiles were evaporated in vacuo and the residue was dissolved in ethyl acetate (100 ml) and filtered through silicagel (100 ml) using ethyl acetate as eluent. The solvent was evaporated in vacuo and to the residue was added a mixture of ethyl acetate (25 ml) and heptane (25 ml). The precipitate was filtered off and washed with heptane (40 ml), dried in vacuo at 50° C. which afforded 9.0 g (83%) of naphthalene-2-carbothioic acid amide as a solid.

후처리

  1. customThe volatiles were evaporated in vacuo
  2. dissolutionthe residue was dissolved in ethyl acetate (100 ml)
  3. filtrationfiltered through silicagel (100 ml)
  4. customThe solvent was evaporated in vacuo and to the residue
  5. additionwas added
  6. additiona mixture of ethyl acetate (25 ml) and heptane (25 ml)
  7. filtrationThe precipitate was filtered off
  8. washwashed with heptane (40 ml)
  9. customdried in vacuo at 50° C. which

출처 및 근거

ORD 기록
ord-dbc03a916e514ef48356c6cd452b4ba0
출처 데이터셋
uspto-grants-2000_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06063800

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