Dimethylamine → (3-(Dimethylamino)propyl)triphenylphosphonium bromide hydrobromide

HRID 1527834노트

반응식

HRID 1527834 반응식
[Br-:1].[Br:2][CH2:3][CH2:4][CH2:5][P+:6]([C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)([C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.[CH3:25][NH:26][CH3:27]>C(O)C.O>[BrH:2].[Br-:1].[CH3:25][N:26]([CH3:27])[CH2:3][CH2:4][CH2:5][P+:6]([C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)([C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1

참가 물질

5

반응물 2

HCID 674DimethylamineHCID 2723862(3-Bromopropyl)triphenylphosphonium bromide

생성물 1

HCID 23651404(3-(Dimethylamino)propyl)triphenylphosphonium bromide hydrobromide수율 82%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

반응 조건

온도
100 °C

실험 절차

To a suspension of 3-bromopropyltriphenylphosphonium bromide (1.0 g, 2.1 mmol) in ethanol (5 mL) was added a solution of 40% dimethylamine in water (3 mL) at room temperature. The mixture was stirred and heated at 100° C. for 30 min in a sealed microwave tube. After the reaction mixture was concentrated under reduced pressure, the solid residue was recrystallized in acetonitrile to afford (3-(dimethylamino)propyl)triphenylphosphonium bromide hydrobromide salt (0.90 g, 82%) as a white solid, and was used in the following step. ESI MS m/z 348.3 (Ph3PCH2CH2CH2NMe2)+.

후처리

  1. concentrationAfter the reaction mixture was concentrated under reduced pressure
  2. customthe solid residue was recrystallized in acetonitrile

출처 및 근거

ORD 기록
ord-26d3e2d863194984a58bd0fb54e1234a
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09090535B2

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