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

HRID 12643

반응식

HRID 12643 반응식
[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

참가 물질

6

반응물 5

HCID 962WaterHCID 3283Diethyl Ether2회HCID 25517Ammonium ChlorideHCID 57839521Dimethylamino-(1,4-dioxaspiro[4.5]dec-8-yl)-acetonitrileHCID 178478191HCID 178478191, 화합물

생성물 1

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

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b624ee5bc34e462b952ecc7a6393457b
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07728028B2

연결된 노트

불러오는 중…