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1,2-Dichloroethane → methyl (2S,4E)-4-methoxyimino-1-[4-(2-methylphenyl)benzoyl]pyrrolidine-2-carboxylate

HRID 457922
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HRID 457922 반응식
[CH3:1][O:2][C:3]([C@@H:5]1[CH2:9][C:8](=[N:10][O:11][CH3:12])[CH2:7][NH:6]1)=[O:4].[CH3:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=1[C:20]1[CH:25]=[CH:24][C:23]([C:26](O)=[O:27])=[CH:22][CH:21]=1.C(Cl)Cl.C(Cl)CCl>CN(C)C1C=CN=CC=1.CN(C=O)C>[CH3:12][O:11]/[N:10]=[C:8]1\[CH2:9][C@@H:5]([C:3]([O:2][CH3:1])=[O:4])[N:6]([C:26]([C:23]2[CH:22]=[CH:21][C:20]([C:15]3[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=3[CH3:13])=[CH:25][CH:24]=2)=[O:27])[CH2:7]\1
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참가 물질

7

반응물 4

HCID 111,2-DichloroethaneHCID 6344DichloromethaneHCID 27598152'-Methyl-biphenyl-4-carboxylic acidHCID 123256627methyl-(2S,4EZ)-4-(methoxyimino)2-pyrrolidinecarboxylate

생성물 1

HCID 10109472methyl (2S,4E)-4-methoxyimino-1-[4-(2-methylphenyl)benzoyl]pyrrolidine-2-carboxylate수율 22%

시약·촉매·용매 2

HCID 14284
4-(Dimethylamino)pyridine
촉매
HCID 6228Dimethylformamide용매

실험 절차

Method A (e.g. methyl (2S,4EZ)-4-4-(methoxyimino-1-[(2′-methyl[1,1′-biphenyl]-4-yl)carbonyl]-2-pyrrolidinecarboxylate): A solution of methyl-(2S,4EZ)-4-(methoxyimino)-2-pyrrolidinecarboxylate (0.564 g, 3.28 mmol), 2′-methyl[1,1′-biphenyl]-4-carboxylic acid (0.765 g, 3.60 mmol) and 4-dimethylaminopyridine (0.880 g, 7.21 mmol) in a 7:3 mixture of DCM and DMF (30 ml) was made. EDC (0.691 mg, 3.60 mmol) was added slowly at 0° C. The reaction mixture was stirred overnight at r.t. It was washed with water (twice 20 ml), dried over MgSO4, filtrated and evaporated in vacuo. The resulting crude product mixture, methyl (2S,4EZ)-4-(methoxyimino)-1-[(2′-methyl[1,1′-biphenyl]-4-yl)carbonyl]-2-pyrrolidinecarboxylate, was purified by flash chromatography, unsing cyclohexane/EtOAc 8:2 as eluent. After several further chromatographies, (E)- and (Z)-isomers could be separated: methyl (2S,4E)-4-(methoxyimino)-1-[(2′-methyl[1,1′-biphenyl]-4-yl)carbonyl]-2-pyrrolidinecarboxylate (261 mg, 22%) was isolated as a colorless powder in 98.3% purity by HPLC, and methyl (2S,4Z)-4-(methoxyimino)-1-[(2′-methyl[1,1′-biphenyl]-4-yl)carbonyl]-2-pyrrolidinecarboxylate (237 mg, 20%) was isolated as a colorless powder in 98.3% purity by HPLC.

후처리

  1. washIt was washed with water (twice 20 ml)
  2. dry with materialdried over MgSO4
  3. filtrationfiltrated
  4. customevaporated in vacuo
  5. customThe resulting crude product mixture, methyl (2S,4EZ)-4-(methoxyimino)-1-[(2′-methyl[1,1′-biphenyl]-4-yl)carbonyl]-2-pyrrolidinecarboxylate, was purified by flash chromatography, unsing cyclohexane/EtOAc 8:2 as eluent
  6. customAfter several further chromatographies, (E)- and (Z)-isomers could be separated

출처 및 근거

ORD 기록
ord-3a8560e12327401a981174c837567654
출처 데이터셋
uspto-grants-2007_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07189754B2

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