Formamide → 4-Fluorophenyl-tolylthiomethylformamide

HRID 233558

반응식

HRID 233558 반응식
[F:1][C:2]1[CH:9]=[CH:8][C:5](C=O)=[CH:4][CH:3]=1.[C:10]1([CH3:17])[C:15]([SH:16])=[CH:14][CH:13]=[CH:12][CH:11]=1.[CH:18]([NH2:20])=[O:19].[C:21]1(C)C=CC=CC=1>CCOC(C)=O.O>[F:1][C:2]1[CH:3]=[CH:4][C:5]([N:20]([CH2:21][S:16][C:15]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[CH3:17])[CH:18]=[O:19])=[CH:8][CH:9]=1

참가 물질

7

반응물 4

HCID 713FormamideHCID 1140Toluene2회HCID 87122-ThiocresolHCID 680234-Fluorobenzaldehyde

생성물 1

HCID 867501664-Fluorophenyl-tolylthiomethylformamide수율 85%

시약·촉매·용매 2

HCID 962Water용매HCID 8857Ethyl Acetate용매

실험 절차

A solution of p-fluorobenzaldehyde (13.1 milliliters (hereinafter mL), 122 millimoles (hereinafter mmol) thiocresol (16.64 grams (hereinafter g), 122 mmol), formamide (15.0 mL, 445 mmol), and toluene (300 mL) were combined and heated to toluene reflux with azeotropic removal of H2O for 18 h. The cooled reaction was diluted with EtOAc (500 mL) and washed with satd aq Na2CO3 (3×100 mL), satd aq NaCl (100 mL), dried (Na2SO4), and concentrated. The residue was triturated with petroleum ether, filtered and dried in vacuo to afford 28.50 g of the title compound as a white solid (85%). melting point (hereinafter top)=119°-120°.

후처리

  1. customThe cooled reaction
  2. washwashed with satd aq Na2CO3 (3×100 mL)
  3. dry with materialdried (Na2SO4)
  4. concentrationconcentrated
  5. customThe residue was triturated with petroleum ether
  6. filtrationfiltered
  7. customdried in vacuo

출처 및 근거

ORD 기록
ord-204d0e7356d54100923539cea2134fac
출처 데이터셋
uspto-grants-1997_01
특허 번호
US05593992

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