Phosphoric Acid → HCID 14127108、化合物

HRID 1197141ノート

反応式

HRID 1197141 の反応式
[S:1]1[CH:5]=[CH:4][CH:3]=[CH:2]1.[CH3:6][CH:7]1OC(C)OC(C)O1.[CH:15]([C:18]1[CH:26]=[CH:25][C:21]([C:22]([NH2:24])=[O:23])=[CH:20][CH:19]=1)([CH3:17])[CH3:16].P(=O)(O)(O)O>C(O)=O>[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[CH:6]([NH:24][C:22](=[O:23])[C:21]1[CH:25]=[CH:26][C:18]([CH:15]([CH3:17])[CH3:16])=[CH:19][CH:20]=1)[CH3:7]

参加物

6

反応物 4

HCID 1004Phosphoric AcidHCID 8030ThiopheneHCID 31264ParaldehydeHCID 69277Benzamide, 4-(1-methylethyl)-

生成物 1

HCID 14127108HCID 14127108、化合物収率 229.4%

試薬・触媒・溶媒 1

HCID 284Formic Acid溶媒

実験手順

Thiophene (42 g, 0.5 mol), paraldehyde (4.4 g, 0.033 mole) and 4-isopropylbenzamide (16.3 g, 0.1 mol) were added to a mixture of formic acid (40 ml) and 85% phosphoric acid (20 ml) and stirred at a room temperature for three hours. The reaction mixture was extracted with water (70 ml). An organic phase was washed with water (30 ml) and evaporated to dryness with a rotary evaporator. A residue was recrystallized from carbon tetrachloride/petroleum benzine (1:2) to obtain the entitled compound (20.7 g) as a colorless crystal. Yield: 75.8%. Melting point: 100° C.

後処理

  1. extractionThe reaction mixture was extracted with water (70 ml)
  2. washAn organic phase was washed with water (30 ml)
  3. customevaporated to dryness with a rotary evaporator
  4. customA residue was recrystallized from carbon tetrachloride/petroleum benzine (1:2)

出典と根拠

ORDレコード
ord-685f28aec2024f269ada8375a4cdc24c
出典データセット
uspto-grants-1992_05
特許番号
US05117000

反応ノート

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