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Phthalimide → HCID 20468458, 화합물

HRID 1903246
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HRID 1903246 반응식
N(C(OCC)=O)=NC(OCC)=O.[F:13][CH:14]([F:27])[CH:15]([NH:19][CH2:20][C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)[CH2:16][CH2:17]O.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[C:47]1(=[O:57])[NH:51][C:50](=[O:52])[C:49]2=[CH:53][CH:54]=[CH:55][CH:56]=[C:48]12>O1CCCC1.C(OCC)(=O)C.C1CCCCC1>[F:13][CH:14]([F:27])[CH:15]([NH:19][CH2:20][C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)[CH2:16][CH2:17][N:51]1[C:50](=[O:52])[C:49]2=[CH:53][CH:54]=[CH:55][CH:56]=[C:48]2[C:47]1=[O:57]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 6809PhthalimideHCID 11776TriphenylphosphineHCID 220568ethyl N-ethoxycarbonyliminocarbamateHCID 204684403-(Benzylamino)-4,4-difluorobutan-1-OL

생성물 1

HCID 20468458HCID 20468458, 화합물수율 65%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran
용매
2회
HCID 21867204Cyclohexane ethylacetate용매

실험 절차

A solution of diethyl azodicarboxylate (0.639 g, 3.65 mM), in anhydrous tetrahydrofuran (5 ml) is added, dropwise, over a period of 0.5 hours, at room temperature to a mixture of 4,4-difluoro-3-benzylamino-butanol (0.790 g, 3.65 mM) prepared as in Step C, triphenylphosphine (0.962 g, 3.65 mM), and phthalimide (0.540 g, 3.65 mM) in tetrahydrofuran (20 ml). After stirring for 2.5 hours at room temperature, the solvent is evaporated in vacuo. The residue is taken off in benzene and the solution filtered. The solid is washed three time with benzene. The filtrate is evaporated to dryness; the residue is taken off in diethyl ether. Filtration and evaporation of the solvent in vacuo yields a yellow oil. The expected phthalimide is isolated by column chromatography (medium pressure silica gel chromatography technique, ethyl acetate/cyclohexane 2:8): 0.800 g (yield 65%).

후처리

  1. customthe solvent is evaporated in vacuo
  2. filtrationthe solution filtered
  3. washThe solid is washed three time with benzene
  4. customThe filtrate is evaporated to dryness
  5. filtrationFiltration and evaporation of the solvent in vacuo
  6. customyields a yellow oil

출처 및 근거

ORD 기록
ord-bc961804a5bb49fe8baa0076d3db5c30
출처 데이터셋
uspto-grants-1984_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04435425

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