Water → 5-Bromo-2-(2-pyrrolidin-1-ylethoxy)benzylamine
반응식
C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[N:20]([CH2:23][C:24]1[CH:37]=[C:36]([Br:38])[CH:35]=[CH:34][C:25]=1[O:26][CH2:27][CH2:28][N:29]1[CH2:33][CH2:32][CH2:31][CH2:30]1)=[N+]=[N-].O>C1COCC1>[Br:38][C:36]1[CH:35]=[CH:34][C:25]([O:26][CH2:27][CH2:28][N:29]2[CH2:33][CH2:32][CH2:31][CH2:30]2)=[C:24]([CH:37]=1)[CH2:23][NH2:20]참가 물질
5
실험 절차
0.66 g (2.50 mmol) of triphenylphosphine was added to a solution of 0.40 g (1.23 mmol) 1-[2-(2-azidomethyl-4-bromophenoxy)ethyl]pyrrolidine in 5 mL of THF and the mixture was stirred for 30 minutes at RT. Water was added and the aqueous phase was exhaustively extracted with DCM. The combined organic extracts were dried over magnesium sulfate and evaporated down in vacuo. Yield: 0.185 g (50% of theoretical); C13H19BrN2O (M=299.207); calc.: molpeak (M+H)+: 299/301 (Br); found: molpeak (M+H)+: 299/301 (Br); HPLC-MS: 1.38 minutes (method A).
후처리
- extractionthe aqueous phase was exhaustively extracted with DCM
- dry with materialThe combined organic extracts were dried over magnesium sulfate
- customevaporated down in vacuo
- custom1.38 minutes (method A)
출처 및 근거
- ORD 기록
- ord-7cb3bb0020624d43912b34a8c10b5490
- 출처 데이터셋
- uspto-grants-2009_09
- 특허 번호
- US07592358B2
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