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Ethyl 4-oxocyclohexanecarboxylate → HCID 18340695, 화합물

HRID 714511
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HRID 714511 반응식
[Cl-].[Li+].C(OP([CH2:11][C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13])(OCC)=O)C.O=[C:20]1[CH2:25][CH2:24][CH:23]([C:26]([O:28][CH2:29][CH3:30])=[O:27])[CH2:22][CH2:21]1>CC#N>[C:15]([O:14][C:12](=[O:13])[CH:11]=[C:20]1[CH2:25][CH2:24][CH:23]([C:26]([O:28][CH2:29][CH3:30])=[O:27])[CH2:22][CH2:21]1)([CH3:16])([CH3:17])[CH3:18]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 317638Ethyl 4-oxocyclohexanecarboxylateHCID 433294Lithium ChlorideHCID 2773685tert-Butyl diethylphosphonoacetate

생성물 1

HCID 18340695HCID 18340695, 화합물수율 62.1%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

To a suspension of anhydrous lithium chloride (1.9 g, 45 mmol) in MeCN (100 ml) was added tert-butyl 2-(diethoxyphosphoryl)acetate (7.6 g, 30 mmol) at room temperature. The mixture was stirred for 30 min. TEA (6.4 ml, 45 mmol) was added and the mixture was stirred for another 30 min. Ethyl 4-oxocyclohexanecarboxylate (5.1 g, 30 mmol) was added and the mixture was stirred overnight. The precipitate was filtered off and the filtrate was concentrated to afford brown oil, which was purified by silica gel column (PE:EtOAc=10:1) to afford product (5 g, 62%).

후처리

  1. stirringthe mixture was stirred for another 30 min
  2. stirringthe mixture was stirred overnight
  3. filtrationThe precipitate was filtered off
  4. concentrationthe filtrate was concentrated
  5. customto afford brown oil, which
  6. customwas purified by silica gel column (PE:EtOAc=10:1)

출처 및 근거

ORD 기록
ord-d6bc09e0770f4cd694958a3123fba500
출처 데이터셋
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09187447B2

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