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Triphenylphosphine → HCID 178498280, 화합물

HRID 1787936
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HRID 1787936 반응식
[F:1][CH2:2][CH2:3][O:4][C:5]1[CH:14]=[CH:13][C:8]([C:9]([O:11][CH3:12])=[O:10])=[C:7]([OH:15])[CH:6]=1.[C:16]([O:20][C:21]([NH:23][C@H:24]1[CH2:29][CH2:28][C@H:27](O)[CH2:26][CH2:25]1)=[O:22])([CH3:19])([CH3:18])[CH3:17].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.N(C(OCC)=O)=NC(OCC)=O>C1COCC1.CCCCCC.C(OCC)(=O)C>[C:16]([O:20][C:21]([NH:23][C@@H:24]1[CH2:29][CH2:28][C@H:27]([O:15][C:7]2[CH:6]=[C:5]([O:4][CH2:3][CH2:2][F:1])[CH:14]=[CH:13][C:8]=2[C:9]([O:11][CH3:12])=[O:10])[CH2:26][CH2:25]1)=[O:22])([CH3:19])([CH3:17])[CH3:18]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 11776TriphenylphosphineHCID 220568ethyl N-ethoxycarbonyliminocarbamateHCID 10420774Methyl 4-(2-Fluoroethoxy)-2-hydroxybenzoateHCID 178418329HCID 178418329, 화합물

생성물 1

HCID 178498280HCID 178498280, 화합물수율 71.7%

시약·촉매·용매 3

HCID 8028
Tetrahydrofuran
용매
2회
HCID 8058Hexane용매
HCID 8857Ethyl Acetate용매

실험 절차

Using a procedure similar to that of Example 6-D, methyl 4-(2-fluoroethoxy)-2-hydroxybenzoate (5.0 g, 24.75 mmol), trans-4-tert-butoxycarbonylaminocyclohexanol (5.02 g, 24.75 mmol), and triphenylphosphine (1.2 equivalents) in THF (125 mL) is treated with diethyl azodicarboxylate (1.3 equivalents) in THF (25 mL). After having stirred overnight at room temperature, the reaction mixture was heated 8 h at 40-50° C., then stirred overnight at room temperature. The crude product was isolated by elution from silica gel with a gradient of 0 to 40% ethyl acetate in hexane to afford crude methyl 2-(cis-4-tert-butoxycarbonylaminocyclohexyloxy)-4-(2-fluoroethoxy)benzoate (7.30 g), which is used without further purification.

후처리

  1. temperaturethe reaction mixture was heated 8 h at 40-50° C.
  2. stirringstirred overnight at room temperature

출처 및 근거

ORD 기록
ord-0fe4a2024130415982a1cf7bb40535a2
출처 데이터셋
uspto-grants-2009_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07511066B2

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