Triethylamine → 1-Methyl-beta-oxo-alpha-(2,6-dichlorophenylcarbamoyl)-2-pyrrolpropionitrile

HRID 127592

反応式

HRID 127592 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[N:9]=[C:10]=[O:11].[CH3:12][N:13]1[CH:17]=[CH:16][CH:15]=[C:14]1[C:18](=[O:22])[CH2:19][C:20]#[N:21].C(N(CC)CC)C>C1(C)C=CC=CC=1>[CH3:12][N:13]1[CH:17]=[CH:16][CH:15]=[C:14]1[C:18](=[O:22])[CH:19]([C:10](=[O:11])[NH:9][C:3]1[C:2]([Cl:1])=[CH:7][CH:6]=[CH:5][C:4]=1[Cl:8])[C:20]#[N:21]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 6045371,3-Dichloro-2-isocyanatobenzeneHCID 27771703-(1-Methyl-1H-pyrrol-2-yl)-3-oxopropanenitrile

生成物 1

HCID 202854251-Methyl-beta-oxo-alpha-(2,6-dichlorophenylcarbamoyl)-2-pyrrolpropionitrile

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

To the filtered solution of 4.4 g of 2,6-dichlorophenylisocyanate in 30 ml of toluene is added 2.5 g of 1-methyl-β-oxo-2-pyrrolpropionitrile and 2.1 g of triethylamine while stirring. The mixture is allowed to stand overnight at room temperature, whereupon it is filtered. The solids are washed with toluene and diethyl ether, taken up in 50 ml of methanol and the solution poured into the mixture of 6 ml of 5 N hydrochloric acid and 300 ml of water. The crystals formed are collected, washed with water, dried, triturated with ethanol, and recrystallized from methanol, to yield the 1-methyl-β-oxo-α-(2,6-dichlorophenylcarbamoyl)-2-pyrrolpropionitrile melting at 196°-199°.

後処理

  1. filtrationis filtered
  2. washThe solids are washed with toluene and diethyl ether
  3. additionthe solution poured into the mixture of 6 ml of 5 N hydrochloric acid and 300 ml of water
  4. customThe crystals formed
  5. customare collected
  6. washwashed with water
  7. customdried
  8. customtriturated with ethanol
  9. customrecrystallized from methanol

出典と根拠

ORDレコード
ord-aa5d06143fbb44aea1ef74dd2804a70f
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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