Diisopropylethylamine → Ethylbis(propan-2-yl)amine hydrochloride

HRID 924008ノート

反応式

HRID 924008 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].[CH3:23][NH:24][CH2:25][CH2:26][CH2:27][OH:28].[CH3:29][CH2:30][N:31]([CH:35]([CH3:37])[CH3:36])[CH:32]([CH3:34])[CH3:33]>CC(O)C>[Br:1][C:2]1[C:3]([N:24]([CH2:25][CH2:26][CH2:27][OH:28])[CH3:23])=[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].[CH3:29][CH2:30][N:31]([CH:35]([CH3:37])[CH3:36])[CH:32]([CH3:34])[CH3:33].[ClH:22]

参加物

6

反応物 3

HCID 81531DiisopropylethylamineHCID 101489863-(Methylamino)-1-propanolHCID 867025955-bromo-6-chloro-N-(4-(trifluoromethoxy)phenyl)nicotinamide

生成物 2

HCID 10997398Ethylbis(propan-2-yl)amine hydrochlorideHCID 899063685-bromo-6-((3-hydroxypropyl)(methyl)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, 237 mg, 0.60 mmol), 3-(methylamino)propan-1-ol (64 mg, 0.72 mmol), iPrOH (2.4 mL) and DIPEA (0.205 mL, 0.155 g, 1.2 mmol) were subjected to MW irradiation at 140° C. for 3 h. 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 in an equimolar mixture with DIPEA hydrochloride. LC-MS (Condition 5) tR=1.18 min, m/z=448.0 [M+H]+, m/z=446.0 [M−H]−.

後処理

  1. customwere subjected to MW irradiation at 140° C. for 3 h
  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-c67f6c83708f43728cf52cebc9672a9c
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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