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Phenethylamine → HCID 18628782, 화합물

HRID 1060734
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HRID 1060734 반응식
Cl[C:2]([CH:4]([CH2:10][CH:11]1[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]1)[C:5]([O:7][CH2:8][CH3:9])=[O:6])=[O:3].[CH2:17]([NH2:25])[CH2:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.CN1CCOCC1>C(OCC)(=O)C>[CH:11]1([CH2:10][CH:4]([C:2]([NH:25][CH2:17][CH2:18][C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)=[O:3])[C:5]([O:7][CH2:8][CH3:9])=[O:6])[CH2:16][CH2:15][CH2:14][CH2:13][CH2:12]1
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참가 물질

5

반응물 3

HCID 1001PhenethylamineHCID 79724-MethylmorpholineHCID 18628711HCID 18628711, 화합물

생성물 1

HCID 18628782HCID 18628782, 화합물수율 41.7%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매2회

실험 절차

A mixture of ethyl 2-chlorocarbonyl-3-cyclohexylpropionate (2.65 mmol), phenethylamine (0.376 mL, 3 mmol) and N-methylmorpholine (0.44 mL, 4 mmol) in ethyl acetate (6 mL) was cooled to between −20 and −10° C. and stirred for 15 minutes. The mixture was allowed to warm to room temperature, stirred for approximately 12 hours and then diluted with ethyl acetate (5 mL) and ice (5 mL). The organic layer was separated, washed with cold 0.05 N hydrochloric acid, sodium bicarbonate solution and brine, dried (MgSO4) and concentrated to provide ethyl 2-cyclohexylmethyl-N-phenethylmalonamate (366 mg, 1.106 mmol).

후처리

  1. temperaturewas cooled to between −20 and −10° C.
  2. stirringstirred for approximately 12 hours
  3. customThe organic layer was separated
  4. washwashed with cold 0.05 N hydrochloric acid, sodium bicarbonate solution and brine
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-2eeb6908940848a5b79841cfbc11c8a3
출처 데이터셋
uspto-grants-2003_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06525036B2

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