3-Amino-1-propanol → Ethylbis(propan-2-yl)amine hydrochloride

HRID 924003노트

반응식

HRID 924003 반응식
[Br:1][C:2]1[C:3]([Cl:22])=[N:4][CH:5]=[C:6]([CH:21]=1)[C:7]([NH:9][C:10]1[CH:15]=[CH:14][C:13]([O:16][C:17]([F:20])([F:19])[F:18])=[CH:12][CH:11]=1)=[O:8].[NH2:23][CH2:24][CH2:25][CH2:26][OH:27].[CH3:28][CH2:29][N:30]([CH:34]([CH3:36])[CH3:35])[CH:31]([CH3:33])[CH3:32]>CC(O)C>[Br:1][C:2]1[C:3]([NH:23][CH2:24][CH2:25][CH2:26][OH:27])=[N:4][CH:5]=[C:6]([CH:21]=1)[C:7]([NH:9][C:10]1[CH:15]=[CH:14][C:13]([O:16][C:17]([F:20])([F:19])[F:18])=[CH:12][CH:11]=1)=[O:8].[CH3:28][CH2:29][N:30]([CH:34]([CH3:36])[CH3:35])[CH:31]([CH3:33])[CH3:32].[ClH:22]

참가 물질

6

반응물 3

HCID 90863-Amino-1-propanolHCID 81531DiisopropylethylamineHCID 867025955-bromo-6-chloro-N-(4-(trifluoromethoxy)phenyl)nicotinamide

생성물 2

HCID 10997398Ethylbis(propan-2-yl)amine hydrochlorideHCID 899067795-bromo-6-((3-hydroxypropyl)amino)-N-(4-(trifluoromethoxy)phenyl)nicotinamide

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

A mixture of 5-bromo-6-chloro-N-(4-(trifluoromethoxy)phenyl)nicotinamide (Stage 12.2, 198 mg, 0.50 mmol), 3-aminopropan-1-ol (45 mg, 0.60 mmol), iPrOH (2 mL) and DIPEA (0.171 mL, 0.129 g, 1.0 mmol) were subjected to MW irradiation at 140° C. for 150 min. The vial was cooled to RT and the RM was evaporated to dryness under reduced pressure. No further purification was required to afford the title compound as an equimolar mixture with DIPEA hydrochloride. UPLC-MS (Condition 8) tR=1.46 min, m/z=434.0 [M+H]+, m/z=432.1 [M−H]−.

후처리

  1. customwere subjected to MW irradiation at 140° C. for 150 min
  2. customthe RM was evaporated to dryness under reduced pressure
  3. customNo further purification

출처 및 근거

ORD 기록
ord-2e2065cb160b4fd39ba24d8342d28327
출처 데이터셋
uspto-grants-2016_03
특허 번호
US09278981B2

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