Ammonia → N2-methyl-N-[3-(triphenylphosphonio)propyl]glycinamide chloride

HRID 58335노트

반응식

HRID 58335 반응식
C(O[C:6]([N:8](C)[CH2:9][C:10]([NH:12][CH2:13][CH2:14][CH2:15][P+:16]([C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1)([C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)=[O:11])=O)(C)(C)C.[Cl-:36].Cl.C(OCC)C.N>C(Cl)Cl.CO>[CH3:6][NH:8][CH2:9][C:10]([NH:12][CH2:13][CH2:14][CH2:15][P+:16]([C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=1)([C:23]1[CH:24]=[CH:25][CH:26]=[CH:27][CH:28]=1)[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)=[O:11].[Cl-:36]

참가 물질

7

반응물 4

HCID 222AmmoniaHCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 131737005N2-(tert-butoxycarbonyl)-N2-methyl-N-[3-(triphenylphosphonio)propyl]glycinamide chloride

생성물 1

HCID 131737006N2-methyl-N-[3-(triphenylphosphonio)propyl]glycinamide chloride수율 100%

시약·촉매·용매 2

HCID 887Methanol용매2회HCID 6344Dichloromethane용매

실험 절차

To a solution of N2-(tert-butoxycarbonyl)-N2-methyl-N-[3-(triphenylphosphonio)propyl]glycinamide chloride (7.6 g, 14 mol) in methylene chloride (38 mL) and methanol (4.2 mL) was added 2.0 M HCl in diethyl ether (16 mL, 32 mmol), and the mixture was stirred overnight at room temperature. The solution was cooled to 0° C. and treated with 7 M ammonia in methanol (6.0 mL, 42 mmol), giving an immediate white precipitate. After 30 minutes, the slurry was filtered and the flask and filter cake were rinsed with methylene chloride (68 mL). The filtrate was concentrated to give the title compound (6.2 g, 100%) as a crude white solid.

후처리

  1. temperatureThe solution was cooled to 0° C.
  2. customgiving an immediate white precipitate
  3. waitAfter 30 minutes
  4. filtrationthe slurry was filtered
  5. filtrationthe flask and filter cake
  6. washwere rinsed with methylene chloride (68 mL)
  7. concentrationThe filtrate was concentrated

출처 및 근거

ORD 기록
ord-dd5c36bf369e4300a33843e92a619a23
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09434753B2

반응 노트

불러오는 중…