Hydrochloric Acid → Methyl 3-(2-trichloroacetylpyrrol-1-yl)benzoate

HRID 399824ノート

反応式

HRID 399824 の反応式
[Cl:1][C:2]([Cl:7])([Cl:6])[C:3](Cl)=[O:4].[N:8]1([C:13]2[CH:14]=[C:15]([CH:20]=[CH:21][CH:22]=2)[C:16]([O:18][CH3:19])=[O:17])[CH:12]=[CH:11][CH:10]=[CH:9]1.N1C=CC=CC=1.Cl>ClCCCl.O.C(Cl)(Cl)Cl>[Cl:1][C:2]([Cl:7])([Cl:6])[C:3]([C:12]1[N:8]([C:13]2[CH:14]=[C:15]([CH:20]=[CH:21][CH:22]=2)[C:16]([O:18][CH3:19])=[O:17])[CH:9]=[CH:10][CH:11]=1)=[O:4]

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 1049PyridineHCID 6420Trichloroacetyl chlorideHCID 3322314Methyl 3-(1H-pyrrol-1-yl)benzoate

生成物 1

HCID 18945198Methyl 3-(2-trichloroacetylpyrrol-1-yl)benzoate

試薬・触媒・溶媒 3

HCID 111,2-Dichloroethane溶媒HCID 962Water溶媒HCID 6212Chloroform溶媒

実験手順

Trichloroacetyl chloride (15.5 ml) was added to a mixture of methyl 3-(pyrrol-1-yl)benzoate (14.0 g) and pyridine (16.9 ml) in 1,2-dichloroethane (70 ml) under ice-cooling and the mixture was stirred for 7 days at ambient temperature. The mixture was poured into a mixture of chloroform and water, and the mixture was adjusted to pH 1 with 6N-hydrochloric acid. The separated organic layer was washed with a saturated aqueous sodium bicarbonate solution and water. The mixture was dried over magnesium sulfate and evaporated in vacuo. The residue was triturated with diisopropyl ether to give methyl 3-(2-trichloroacetylpyrrol-1-yl)benzoate (21.23 g).

後処理

  1. temperaturecooling
  2. washThe separated organic layer was washed with a saturated aqueous sodium bicarbonate solution and water
  3. dry with materialThe mixture was dried over magnesium sulfate
  4. customevaporated in vacuo
  5. customThe residue was triturated with diisopropyl ether

出典と根拠

ORDレコード
ord-8bfe52f7eaf74760a8571bf51d2959ac
出典データセット
uspto-grants-1998_10
特許番号
US05824691

反応ノート

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