Water → HCID 69811611, 화합물

HRID 2063724

반응식

HRID 2063724 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([Mg]Br)[CH:6]=[CH:7][CH:8]=1.[CH3:11][N:12]([CH3:35])[C:13]1(C#N)[CH2:18][CH2:17][CH:16]([CH:19]([O:27][CH:28]([O:30][CH2:31][CH3:32])[CH3:29])[CH2:20][C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[CH2:15][CH2:14]1.O.[Cl-].[NH4+]>O1CCCC1>[CH2:31]([O:30][CH:28]([O:27][CH:19]([CH:16]1[CH2:17][CH2:18][C:13]([N:12]([CH3:35])[CH3:11])([C:5]2[CH:6]=[CH:7][CH:8]=[C:3]([O:2][CH3:1])[CH:4]=2)[CH2:14][CH2:15]1)[CH2:20][C:21]1[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=1)[CH3:29])[CH3:32]

참가 물질

6

반응물 4

HCID 962WaterHCID 25517Ammonium ChlorideHCID 698102431-Dimethylamino-4-[1-(1-ethoxy-ethoxy)-2-phenylethyl]cyclohexanecarbonitrileHCID 178490745HCID 178490745, 화합물

생성물 1

HCID 69811611HCID 69811611, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

A 1 M solution of 3-methoxyphenylmagnesium bromide in tetrahydrofuran (9.25 ml, 9.25 mmol) was added dropwise to a solution of 1-dimethylamino-4-[1-(1-ethoxy-ethoxy)-2-phenylethyl]cyclohexanecarbonitrile (1.06 g, 3.1 mmol) in tetrahydrofuran (15 ml), while cooling with ice and under an argon atmosphere. The mixture was stirred at room temperature for 48 h and thereafter water and saturated ammonium chloride solution (10 ml of each) were added. The phases were separated and the aqueous phase was extracted with diethyl ether (3×10 ml). The combined organic phases were dried with sodium sulfate and concentrated i. vac.

후처리

  1. temperaturewhile cooling with ice and under an argon atmosphere
  2. customThe phases were separated
  3. extractionthe aqueous phase was extracted with diethyl ether (3×10 ml)
  4. dry with materialThe combined organic phases were dried with sodium sulfate
  5. concentrationconcentrated i

출처 및 근거

ORD 기록
ord-c2f3f223e4414f83a7715a72e3a49a6c
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08288406B2

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