Water → (4-Chlorophenyl)-(1,4-dioxa-spiro[4.5]dec-8-yl]-dimethylamine

HRID 12643

反応式

HRID 12643 の反応式
[CH3:1][N:2]([CH:4]([CH:7]1CCC2(OCCO2)C[CH2:8]1)[C:5]#N)[CH3:3].[Cl:17][C:18]1[CH:23]=[CH:22][C:21]([Mg]Br)=[CH:20][CH:19]=1.[Cl-].[NH4+].[OH2:28].[CH3:29][CH2:30][O:31][CH2:32][CH3:33]>>[Cl:17][C:18]1[CH:23]=[CH:22][C:21]([CH2:1][N:2]([CH:4]2[CH2:7][CH2:8][C:30]3([O:28][CH2:33][CH2:32][O:31]3)[CH2:29][CH2:5]2)[CH3:3])=[CH:20][CH:19]=1

参加物

6

反応物 5

HCID 962WaterHCID 3283Diethyl Ether2 回HCID 25517Ammonium ChlorideHCID 57839521Dimethylamino-(1,4-dioxaspiro[4.5]dec-8-yl)-acetonitrileHCID 178478191HCID 178478191、化合物

生成物 1

HCID 79120490(4-Chlorophenyl)-(1,4-dioxa-spiro[4.5]dec-8-yl]-dimethylamine

実験手順

A solution of the aminonitrile 6 (22.43 g, 100 mmole) in absolute ether (100 ml) was added to a 1M solution of 4-chlorophenyl magnesium bromide in ether (200 ml, 200 mmole) under argon and while cooling with ice, and stirred for 20 hours at RT. To work up the reaction mixture, saturated ammonium chloride solution (100 ml) and water (100 ml) were added while cooling with ice, and the mixture was extracted with diethyl ether (3×100 ml). The organic phase was washed with water and saturated sodium chloride solution, dried, and concentrated by evaporation.

後処理

  1. temperaturewhile cooling with ice
  2. additionwere added
  3. temperaturewhile cooling with ice
  4. extractionthe mixture was extracted with diethyl ether (3×100 ml)
  5. washThe organic phase was washed with water and saturated sodium chloride solution
  6. customdried
  7. concentrationconcentrated by evaporation

出典と根拠

ORDレコード
ord-b624ee5bc34e462b952ecc7a6393457b
出典データセット
uspto-grants-2010_06
特許番号
US07728028B2

関連ノート

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