Diethyl Ether → HCID 20442929、化合物

HRID 647563ノート

反応式

HRID 647563 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-41e1841da62f47828fdbf89f464447b7
出典データセット
uspto-grants-1983_10
特許番号
US04409241

反応ノート

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