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Phthalimide → N-[2-[1-[2-(tert-Butyldiphenylsiloxy)ethyl]cyclohexyl]ethyl]-phthalimide

HRID 2223870
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HRID 2223870 반응식
[O:1]([CH2:19][CH2:20][C:21]1([CH2:27][CH2:28]O)[CH2:26][CH2:25][CH2:24][CH2:23][CH2:22]1)[Si:2]([C:15]([CH3:18])([CH3:17])[CH3:16])([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[C:30]1(=[O:40])[NH:34][C:33](=[O:35])[C:32]2=[CH:36][CH:37]=[CH:38][CH:39]=[C:31]12.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.N(C(OCC)=O)=NC(OCC)=O>O1CCCC1>[O:1]([CH2:19][CH2:20][C:21]1([CH2:27][CH2:28][N:34]2[C:30](=[O:40])[C:31]3=[CH:39][CH:38]=[CH:37][CH:36]=[C:32]3[C:33]2=[O:35])[CH2:22][CH2:23][CH2:24][CH2:25][CH2:26]1)[Si:2]([C:15]([CH3:18])([CH3:17])[CH3:16])([C:9]1[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 6809PhthalimideHCID 11776TriphenylphosphineHCID 220568ethyl N-ethoxycarbonyliminocarbamateHCID 574278602-[1-(2-tert-Butyldiphenylsiloxyethyl)cyclohexyl]ethanol

생성물 1

HCID 59714868N-[2-[1-[2-(tert-Butyldiphenylsiloxy)ethyl]cyclohexyl]ethyl]-phthalimide수율 66.8%

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매

실험 절차

2-[1-[2-(tert-Butyldiphenylsiloxy)ethyl]cyclohexyl]ethanol (1.23 g), phthalimide (530 mg) and triphenylphosphine (1.10 g) were dissolved in tetrahydrofuran (15 mL) and stirred for 20 minutes. Diethyl azocarboxylate (0.57 mL) was then added to the solution, and it was stirred at room temperature for 18 hours. The solvent was distilled off under reduced pressure, and the resulting residue was purified by chromatography (silica gel, 15-20% ethyl acetate:hexane) to give the title compound (1.08 g).

후처리

  1. stirringwas stirred at room temperature for 18 hours
  2. distillationThe solvent was distilled off under reduced pressure
  3. customthe resulting residue was purified by chromatography (silica gel, 15-20% ethyl acetate:hexane)

출처 및 근거

ORD 기록
ord-e50cafab06694e1d853ebdf3bf76fb8d
출처 데이터셋
uspto-grants-2008_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07375115B2

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