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

HRID 924003ノート

反応式

HRID 924003 の反応式
[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]

参加物

6

反応物 3

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

生成物 2

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

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

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]−.

後処理

  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

出典と根拠

ORDレコード
ord-2e2065cb160b4fd39ba24d8342d28327
出典データセット
uspto-grants-2016_03
特許番号
US09278981B2

反応ノート

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