Diethyl Ether → HCID 20442929、化合物

HRID 1702228ノート

反応式

HRID 1702228 の反応式
[CH3:1][NH:2][C:3]1[CH:17]=[CH:16][C:15]([Cl:18])=[CH:14][C:4]=1[C:5]([C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[Cl:13])=[O:6].[Br:19][CH2:20][C:21](Br)=[O:22].C(OCC)C>C(OCC)(=O)C>[CH3:1][N:2]([C:21](=[O:22])[CH2:20][Br:19])[C:3]1[CH:17]=[CH:16][C:15]([Cl:18])=[CH:14][C:4]=1[C:5](=[O:6])[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[Cl:13]

参加物

5

反応物 3

HCID 3283Diethyl EtherHCID 21833Benzophenone, 2',5-dichloro-2-methylamino-HCID 61147Bromoacetyl bromide

生成物 1

HCID 20442929HCID 20442929、化合物収率 81%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of 56 g of 2-methylamino-2',5-dichlorobenzophenone in 400 cc of ethyl acetate there are added an equal volume of ice and then 23 cc of bromoacetylbromide. After stirring overnight at room temperature, 300 cc of ethyl ether are added. The solvent layer is decanted, washed with 2 N caustic soda, and then washed with water until neutral. It is then dried over sodium sulfate, filtered, and evaporated to dryness. The residue is treated with petroleum ether and then recrystallized from ethyl acetate. In this way there are obtained 65 g of crystals; yield: 81%.

後処理

  1. customThe solvent layer is decanted
  2. washwashed with 2 N caustic soda
  3. washwashed with water until neutral
  4. dry with materialIt is then dried over sodium sulfate
  5. filtrationfiltered
  6. customevaporated to dryness
  7. additionThe residue is treated with petroleum ether
  8. customrecrystallized from ethyl acetate

出典と根拠

ORDレコード
ord-d03bc96433394a8faa66e8de7b6d672a
出典データセット
uspto-grants-1983_04
特許番号
US04380667

反応ノート

読み込み中…