Formamide → 4-Fluorophenyl-tolylthiomethylformamide

HRID 233529

反応式

HRID 233529 の反応式
[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

参加物

7

反応物 4

HCID 713FormamideHCID 1140Toluene2 回HCID 87122-ThiocresolHCID 680234-Fluorobenzaldehyde

生成物 1

HCID 867501664-Fluorophenyl-tolylthiomethylformamide収率 85%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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 said aq Na2CO3 (3×100 mL), said 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 mp) =119°-120°.

後処理

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

出典と根拠

ORDレコード
ord-5fb1c4d1b94544289666217774b8f0bb
出典データセット
uspto-grants-1997_01
特許番号
US05593991

関連ノート

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