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Tetrahydrofuran → HCID 68530764, 화합물

HRID 1967421
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HRID 1967421 반응식
[NH2:1][N:2]1[C:6](=[O:7])[C:5]2=[CH:8][CH:9]=[CH:10][CH:11]=[C:4]2[C:3]1=[O:12].O1CCCC1.[CH3:18][C:19]([CH3:29])([CH2:27][CH3:28])[CH:20]([CH2:23][C:24](=O)[CH3:25])[CH:21]=O>Cl.C(OCC)(=O)C>[CH3:18][C:19]([C:20]1[CH:23]=[C:24]([CH3:25])[N:1]([N:2]2[C:3](=[O:12])[C:4]3[C:5](=[CH:8][CH:9]=[CH:10][CH:11]=3)[C:6]2=[O:7])[CH:21]=1)([CH3:29])[CH2:27][CH3:28]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 8028TetrahydrofuranHCID 74645N-AminophthalimideHCID 86642084HCID 86642084, 화합물

생성물 1

HCID 68530764HCID 68530764, 화합물수율 77.6%

시약·촉매·용매 2

HCID 313Hydrochloric Acid촉매HCID 8857Ethyl Acetate용매

실험 절차

N-aminophthalimide (476 mg) and 5N hydrochloric acid (5 drops) were added to the tetrahydrofuran solution (20 mL) of the compound prepared in Example 54 (1 g). The reaction mixture was stirred for 20 minutes under argon gas atmosphere. Ethyl acetate (100 mL) was added to the reaction mixture. The reaction mixture was washed by a saturated aqueous solution of sodium bicarbonate and a saturated aqueous solution of sodium chloride. The organic layer was dried with anhydrous sodium sulfate, and concentrated under reduced pressure. The obtained residue was purified by column chromatography on silica gel (Yamazen corporation, high flash 2 L, n-hexane→ethyl acetate/n-hexane=1/4) to obtain the title compound (675 mg) having the following physical data.

후처리

  1. washThe reaction mixture was washed by a saturated aqueous solution of sodium bicarbonate
  2. dry with materialThe organic layer was dried with anhydrous sodium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customThe obtained residue was purified by column chromatography on silica gel (Yamazen corporation, high flash 2 L, n-hexane→ethyl acetate/n-hexane=1/4)

출처 및 근거

ORD 기록
ord-9256487772b84d7da862fb89310362a6
출처 데이터셋
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08420810B2

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