Water → HCID 69811611、化合物

HRID 2063724

反応式

HRID 2063724 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

HCID 69811611HCID 69811611、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c2f3f223e4414f83a7715a72e3a49a6c
出典データセット
uspto-grants-2012_10
特許番号
US08288406B2

関連ノート

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