4-Fluorophenyl isocyanate → 1-Methyl-beta-oxo-alpha-(p-fluorophenylcarbamoyl)-2-pyrrolpropionitrile

HRID 127586

反応式

HRID 127586 の反応式
[CH3:1][N:2]1[CH:6]=[CH:5][CH:4]=[C:3]1[C:7](=[O:11])[CH2:8][C:9]#[N:10].[F:12][C:13]1[CH:18]=[CH:17][C:16]([N:19]=[C:20]=[O:21])=[CH:15][CH:14]=1>C1(C)C=CC=CC=1.C(N(CC)CC)C>[CH3:1][N:2]1[CH:6]=[CH:5][CH:4]=[C:3]1[C:7](=[O:11])[CH:8]([C:20](=[O:21])[NH:19][C:16]1[CH:17]=[CH:18][C:13]([F:12])=[CH:14][CH:15]=1)[C:9]#[N:10]

参加物

5

反応物 2

HCID 709554-Fluorophenyl isocyanateHCID 27771703-(1-Methyl-1H-pyrrol-2-yl)-3-oxopropanenitrile

生成物 1

HCID 202854081-Methyl-beta-oxo-alpha-(p-fluorophenylcarbamoyl)-2-pyrrolpropionitrile

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 8471Triethylamine溶媒

実験手順

To the suspension of 4.0 g of 1-methyl-β-oxo-2-pyrrolpropionitrile in 70 ml of toluene and 3.2 g of triethylamine, 3.7 g of p-fluorophenylisocyanate are added while stirring. The mixture is warmed on the steam cone until dissolution and the red-brown solution is allowed to stand overnight at room temperature. It is evaporated on the steam cone, the residue taken up in methanol and the solution poured into the mixture of 8 ml of 5 N hydrochloric acid and 300 ml of water. The precipitated crystals are collected, washed with water, dried, triturated with methanol and recrystalllized from ethyl acetate, to yield the 1-methyl-β-oxo-α-(p-fluorophenylcarbamoyl)-2-pyrrolpropionitrile melting at 198°-199°.

後処理

  1. additionare added
  2. temperatureThe mixture is warmed on the steam cone until dissolution
  3. customIt is evaporated on the steam cone
  4. additionthe solution poured into the mixture of 8 ml of 5 N hydrochloric acid and 300 ml of water
  5. customThe precipitated crystals are collected
  6. washwashed with water
  7. customdried
  8. customtriturated with methanol

出典と根拠

ORDレコード
ord-2f64fd19d21947a0b715b1e90e45cedb
出典データセット
uspto-grants-1981_03
特許番号
US04256759

関連ノート

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