Methanamine, N-methoxy-, hydrochloride (1:1) → HCID 21070238, 화합물

HRID 1371541

반응식

HRID 1371541 반응식
[C:1]([NH:8][C@H:9]([C:19]([OH:21])=O)[CH2:10][C:11]1[CH:16]=[CH:15][C:14]([C:17]#[N:18])=[CH:13][CH:12]=1)([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2].CN([C:25]([O:29][N:30]1N=NC2C=CC=C[C:31]1=2)=[N+](C)C)C.[B-](F)(F)(F)F.CCN(C(C)C)C(C)C.Cl.CNOC>C(Cl)Cl>[C:1]([NH:8][CH:9]([CH2:10][C:11]1[CH:12]=[CH:13][C:14]([C:17]#[N:18])=[CH:15][CH:16]=1)[C:19]([N:30]([O:29][CH3:25])[CH3:31])=[O:21])([O:3][C:4]([CH3:5])([CH3:6])[CH3:7])=[O:2]

참가 물질

6

반응물 4

HCID 81138Methanamine, N-methoxy-, hydrochloride (1:1)HCID 81531DiisopropylethylamineHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 7020841N-(tert-Butoxycarbonyl)-4-cyano-L-phenylalanine

생성물 1

HCID 21070238HCID 21070238, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

2 g of (N-Boc)-4-cyanophenylalanine, 2.32 g of TBTU, 2.40 ml of DIPEA and 806 mg of N,O-dimethylhydroxylamine hydrochloride are mixed together in 30 ml of DCM. After stirring for 24 hours at RT, the reaction mixture is concentrated to dryness and the residue is then extracted with EtOAc. The organic phase is washed with a pH 2 buffer solution, a saturated NaHCO3 solution and then a saturated NaCl solution. The expected compound crystallizes from a mixture of isopropyl ether and pentane (1.89 g).

후처리

  1. concentrationthe reaction mixture is concentrated to dryness
  2. extractionthe residue is then extracted with EtOAc
  3. washThe organic phase is washed with a pH 2 buffer solution
  4. customThe expected compound crystallizes from a mixture of isopropyl ether and pentane (1.89 g)

출처 및 근거

ORD 기록
ord-90a6d7c751cc4148b1a4a3cdbb4e6014
출처 데이터셋
uspto-grants-2007_01
특허 번호
US07157454B2

연결된 노트

불러오는 중…