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Triphenylphosphine → HCID 67067087, 화합물

HRID 2074271
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HRID 2074271 반응식
N(C(OCC)=O)=NC(OCC)=O.[OH:13][C:14]1[CH:35]=[CH:34][C:17]([O:18][CH:19]2[CH2:24][CH2:23][N:22]([C:25]([O:27][C:28]3[CH:29]=[N:30][CH:31]=[CH:32][CH:33]=3)=[O:26])[CH2:21][CH2:20]2)=[CH:16][CH:15]=1.[Cl:36][C:37]1[CH:38]=[C:39]([CH:42]=[CH:43][CH:44]=1)[CH2:40]O.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>C(Cl)(Cl)Cl.C1COCC1>[ClH:36].[Cl:36][C:37]1[CH:38]=[C:39]([CH:42]=[CH:43][CH:44]=1)[CH2:40][O:13][C:14]1[CH:35]=[CH:34][C:17]([O:18][CH:19]2[CH2:24][CH2:23][N:22]([C:25]([O:27][C:28]3[CH:29]=[N:30][CH:31]=[CH:32][CH:33]=3)=[O:26])[CH2:21][CH2:20]2)=[CH:16][CH:15]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 11776TriphenylphosphineHCID 701173-Chlorobenzyl alcoholHCID 220568ethyl N-ethoxycarbonyliminocarbamateHCID 670670763-Pyridyl 4-(4-hydroxyphenoxy)-1-piperidinecarboxylate

생성물 1

HCID 67067087HCID 67067087, 화합물수율 24.5%

시약·촉매·용매 2

HCID 6212
Chloroform
용매
HCID 8028Tetrahydrofuran용매

실험 절차

Diethyl azodicarboxylate (0.35 ml, 40% Tol solution) was dropwise added to a THF (5 ml) solution containing 3-pyridyl 4-(4-hydroxyphenoxy)-1-piperidinecarboxylate (160 mg), 3-chlorobenzyl alcohol (110 mg) and triphenylphosphine (200 mg) at 0° C., followed by stirring at room temperature for 24 hours. The reaction solution was diluted with chloroform, washed with aqueous saturated sodium hydrogencarbonate solution, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (eluent: hexane:EtOAc=1:3 (v/v)). The resulting oil was dissolved in EtOAc (5 ml), and 4 M hydrogen chloride/EtOAc solution (1 ml) was added thereto, followed by stirring at room temperature. The solvent was evaporated under reduced pressure, and the precipitated solid was recrystallized from EtOAc/2-propanol to obtain 3-pyridyl 4-{4-[(3-chlorobenzyl)oxy]phenoxy}-1-piperidinecarboxylate hydrochloride (45 mg).

후처리

  1. washwashed with aqueous saturated sodium hydrogencarbonate solution
  2. dry with materialdried over anhydrous magnesium sulfate
  3. customThe solvent was evaporated under reduced pressure
  4. customthe residue was purified by silica gel column chromatography (eluent: hexane:EtOAc=1:3 (v/v))
  5. dissolutionThe resulting oil was dissolved in EtOAc (5 ml)
  6. addition4 M hydrogen chloride/EtOAc solution (1 ml) was added
  7. stirringby stirring at room temperature
  8. customThe solvent was evaporated under reduced pressure
  9. customthe precipitated solid was recrystallized from EtOAc/2-propanol

출처 및 근거

ORD 기록
ord-91c5b379be4b4361bb3f9ea6056f6c1d
출처 데이터셋
uspto-grants-2011_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07919494B2

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