Diethyl Ether → HCID 20442929, 화합물

HRID 647563노트

반응식

HRID 647563 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 20442929HCID 20442929, 화합물수율 81%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

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%.

후처리

  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

출처 및 근거

ORD 기록
ord-41e1841da62f47828fdbf89f464447b7
출처 데이터셋
uspto-grants-1983_10
특허 번호
US04409241

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