1,3-Propanediamine, N1,N1,N3-trimethyl- → Ethylbis(propan-2-yl)amine hydrochloride

HRID 924012ノート

反応式

HRID 924012 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][N:24]([CH3:30])[CH2:25][CH2:26][CH2:27][NH:28][CH3:29].[CH3:31][CH2:32][N:33]([CH:37]([CH3:39])[CH3:38])[CH:34]([CH3:36])[CH3:35]>CC(O)C>[Br:1][C:2]1[C:3]([N:28]([CH2:27][CH2:26][CH2:25][N:24]([CH3:30])[CH3:23])[CH3:29])=[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].[CH3:31][CH2:32][N:33]([CH:37]([CH3:39])[CH3:38])[CH:34]([CH3:36])[CH3:35].[ClH:22]

参加物

6

反応物 3

HCID 783021,3-Propanediamine, N1,N1,N3-trimethyl-HCID 81531DiisopropylethylamineHCID 867025955-bromo-6-chloro-N-(4-(trifluoromethoxy)phenyl)nicotinamide

生成物 2

HCID 10997398Ethylbis(propan-2-yl)amine hydrochlorideHCID 899066305-bromo-6-((3-(dimethylamino)propyl)(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), N1,N1,N3-trimethylpropane-1,3-diamine (84 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 120 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 in an equimolar mixture with DIPEA hydrochloride. UPLC-MS (Condition 8) tR=2.18 min, m/z=475.1 [M+H]+, m/z=473.1 [M−H]−.

後処理

  1. customwere subjected to MW irradiation at 140° C. for 120 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-fa121dfd44c4483ab87ff62a85a53005
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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