HCID 21994134, 화합물 → tert-Butyl 4-(2-(1,3-dioxoisoindolin-2-yl)ethylidene)piperidine-1-carboxylate

HRID 1978308노트

반응식

HRID 1978308 반응식
Br[CH2:2][CH:3]=[C:4]1[CH2:9][CH2:8][N:7]([C:10]([O:12][C:13]([CH3:16])([CH3:15])[CH3:14])=[O:11])[CH2:6][CH2:5]1.[C:17]1(=[O:27])[NH:21][C:20](=[O:22])[C:19]2=[CH:23][CH:24]=[CH:25][CH:26]=[C:18]12.[K]>CN(C)C=O.O>[C:13]([O:12][C:10]([N:7]1[CH2:8][CH2:9][C:4](=[CH:3][CH2:2][N:21]2[C:20](=[O:22])[C:19]3=[CH:23][CH:24]=[CH:25][CH:26]=[C:18]3[C:17]2=[O:27])[CH2:5][CH2:6]1)=[O:11])([CH3:16])([CH3:15])[CH3:14]

참가 물질

5

반응물 2

HCID 21994134HCID 21994134, 화합물HCID 24194345Phthalimide potassium salt

생성물 1

HCID 21993713tert-Butyl 4-(2-(1,3-dioxoisoindolin-2-yl)ethylidene)piperidine-1-carboxylate

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

A solution of 5.775 g (19.900 mM) of tert-butyl 4-(2-bromoethylidene)piperidine-1-carboxylate and 4.05 g (21.9 mM) of potassium phthalimide in 100 ml of N,N-dimethylformamide was stirred at 100° C. for 1 hour. This reaction mixture was poured in water and extracted with 3 portions of ethyl acetate. The pooled organic layer was dried over anhydrous magnesium sulfate (MgSO4) and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=6/1 to 3/1) to provide the title compound.

후처리

  1. extractionextracted with 3 portions of ethyl acetate
  2. dry with materialThe pooled organic layer was dried over anhydrous magnesium sulfate (MgSO4)
  3. distillationthe solvent was distilled off under reduced pressure
  4. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate=6/1 to 3/1)

출처 및 근거

ORD 기록
ord-978f7f91bbf84dbeb46ae15af637ecff
출처 데이터셋
uspto-grants-2001_05
특허 번호
US06235731B1

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