Hydrochloric Acid → 4-(3-Mercaptopyridin-4-yl)benzonitrile

HRID 470382

반응식

HRID 470382 반응식
F[C:2]1[CH:3]=[N:4][CH:5]=[CH:6][C:7]=1[C:8]1[CH:15]=[CH:14][C:11]([C:12]#[N:13])=[CH:10][CH:9]=1.[S-2:16].[Na+].[Na+].Cl>CN(C=O)C>[SH:16][C:2]1[CH:3]=[N:4][CH:5]=[CH:6][C:7]=1[C:8]1[CH:15]=[CH:14][C:11]([C:12]#[N:13])=[CH:10][CH:9]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14804Sodium SulfideHCID 108564354-(3-Fluoropyridin-4-yl)benzonitrile

생성물 1

HCID 679970614-(3-Mercaptopyridin-4-yl)benzonitrile수율 96%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
130 °C

실험 절차

A mixture of 4-(3-fluoropyridin-4-yl)benzonitrile (1.08 g, 5.4 mmol) and sodium sulfide (0.84 g, 10.8 mmol) in DMF (20 mL) was stirred at 130° C. for 0.5 hours. While the reaction was cooled in ice water bath, aqueous HCl (6N, 2.5 mL) was added drop wise with rigorous stirring. The resulting yellow paste was concentrated using rotary evaporation on a water bath (80° C.) to dryness. The resulting yellow solid was extracted with methanol (4×20 mL). The combined extracts were concentrated to dryness to give a yellow solid (1.1 g, 96%).

후처리

  1. concentrationThe resulting yellow paste was concentrated
  2. customevaporation on a water bath (80° C.) to dryness
  3. extractionThe resulting yellow solid was extracted with methanol (4×20 mL)
  4. concentrationThe combined extracts were concentrated to dryness

출처 및 근거

ORD 기록
ord-cc55aeea824d4cfabb0fc277184748da
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08629278B2

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