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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Dabco → HCID 86660140, 화합물

HRID 1423954
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HRID 1423954 반응식
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([OH:8])[C:3]=1[C:9](=[O:11])[CH3:10].[CH3:12][N:13]([CH3:17])[C:14](Cl)=[S:15].C1N2CCN(CC2)C1>CN(C=O)C>[C:9]([C:3]1[C:2]([F:1])=[CH:7][CH:6]=[CH:5][C:4]=1[O:8][C:14](=[S:15])[N:13]([CH3:17])[CH3:12])(=[O:11])[CH3:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 9237DabcoHCID 27871Dimethylthiocarbamoyl chlorideHCID 27373242'-Fluoro-6'-hydroxyacetophenone

생성물 1

HCID 86660140HCID 86660140, 화합물수율 74.9%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

1-(2-Fluoro-6-hydroxy-phenyl)-ethanone (2.5 g, 16.22 mmol) (available from Apollo Scientific) was dissolved in anhydrous DMF (20 mL.) Dimethylthiocarbamoyl chloride (2.2 g, 17.84 mmol) and DABCO (2.0 g, 17.84 mmol) were added sequentially in one portion. The reaction was permitted to stir overnight at ambient temperature. The reaction was quenched by pouring it into a mixture of 1N HCl-ice. The oily residue was extracted with dichloromethane and dried over sodium sulfate. The crude residue was purified by SGC (20% ethyl acetate in hexanes) to provide the title compound (2.93 g.) 1H NMR (200 MHz, CDCl3): δ (ppm)=7.407 (dd, 1H), 7.026 (t, 1H), 6.876 (d, 1H), 3.404 (s, 3H), 3.341 (sd, 3H), 2.58 (d, 3H).

후처리

  1. additionwere added sequentially in one portion
  2. customThe reaction was quenched
  3. additionby pouring it
  4. additioninto a mixture of 1N HCl-ice
  5. extractionThe oily residue was extracted with dichloromethane
  6. dry with materialdried over sodium sulfate
  7. customThe crude residue was purified by SGC (20% ethyl acetate in hexanes)

출처 및 근거

ORD 기록
ord-d649b1691ae745d6bd052f1680639a4d
출처 데이터셋
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08927591B2

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