Succinimide → Methyl 2-[2-(bromomethyl)phenyl]-3-methoxyprop-2-enoate

HRID 3975

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HRID 3975 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8](=[CH:13][O:14][CH3:15])[C:9]([O:11][CH3:12])=[O:10].[Br:16]N1C(=O)CCC1=O.C1(=O)NC(=O)CC1>N(C(C)(C)C#N)=NC(C)(C)C#N.C(Cl)(Cl)(Cl)Cl>[Br:16][CH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8](=[CH:13][O:14][CH3:15])[C:9]([O:11][CH3:12])=[O:10]

참가 물질

6

반응물 3

HCID 11439SuccinimideHCID 67184N-bromobutanimideHCID 435882Methyl 3-methoxy-2-o-tolylacrylate

생성물 1

HCID 53395349Methyl 2-[2-(bromomethyl)phenyl]-3-methoxyprop-2-enoate수율 97.3%

시약·촉매·용매 2

HCID 6547Azobisisobutyronitrile촉매HCID 5943Carbon Tetrachloride용매

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온도
90 °C

실험 절차

20.6 g of the methyl α-(2-methylphenyl)-β-methoxyacrylate obtained as described in method A, 17.65 g of N-bromosuccinimide, 0.2 g of azobisisobutyronitrile and 150 ml of CCl4 are slowly heated to 90° C. and kept at this temperature until all of the succinimide floats on the solvent. The mixture is filtered, the filtrate is evaporated down, and the oil which remains is dissolved in about 5 ml of acetone and brought to crystallization with n-hexane. 27.5 g of colorless crystals of melting point 86°-87° C. are obtained.

후처리

  1. filtrationThe mixture is filtered
  2. customthe filtrate is evaporated down
  3. dissolutionthe oil which remains is dissolved in about 5 ml of acetone
  4. custombrought to crystallization with n-hexane

출처 및 근거

ORD 기록
ord-f360e909fa154e73a99b18eae08d738d
출처 데이터셋
uspto-grants-1988_02
특허 번호
US04723034

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