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Lithium Chloride → HCID 21093754, 화합물

HRID 1349943
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HRID 1349943 반응식
[Br:1][C:2]1[CH:3]=[C:4]([N+:24]([O-:26])=[O:25])[C:5]([O:22]C)=[C:6]([CH:21]=1)[CH:7]=[C:8]1[CH2:13][CH2:12][N:11]([C:14]([O:16][C:17]([CH3:20])([CH3:19])[CH3:18])=[O:15])[CH2:10][CH2:9]1.[Cl-].[Li+]>CN(C)C=O>[Br:1][C:2]1[CH:3]=[C:4]([N+:24]([O-:26])=[O:25])[C:5]([OH:22])=[C:6]([CH:21]=1)[CH:7]=[C:8]1[CH2:9][CH2:10][N:11]([C:14]([O:16][C:17]([CH3:18])([CH3:19])[CH3:20])=[O:15])[CH2:12][CH2:13]1
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참가 물질

4

반응물 2

HCID 433294Lithium ChlorideHCID 21093755HCID 21093755, 화합물

생성물 1

HCID 21093754HCID 21093754, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
120 °C

실험 절차

A mixture of tert-butyl 4-(5-bromo-2-methoxy-3-nitrobenzylidene)piperidine-1-carboxylate (2.5 g, 5.9 mmol) and lithium chloride (1 g) in anhydrous N,N-dimethylformamide was stirred at 120° C. for 4 h. It was allowed to cool to room temperature and evaporated in vacuo. The residue was treated with water (50 mL) and extracted with diethyl ether (2×100 mL). The combined organic layers was washed with water (50 mL) and dried (Na2SO4). Evaporation of solvent gave the title compound as a crude oil (2.1 g).

후처리

  1. temperatureto cool to room temperature
  2. customevaporated in vacuo
  3. additionThe residue was treated with water (50 mL)
  4. extractionextracted with diethyl ether (2×100 mL)
  5. washThe combined organic layers was washed with water (50 mL)
  6. dry with materialdried (Na2SO4)
  7. customEvaporation of solvent

출처 및 근거

ORD 기록
ord-9fc2eb7150994e1ea81f17e381821bce
출처 데이터셋
uspto-grants-2007_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07214674B2

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