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1-Ethylpiperazine → 10-[1-(4-Ethylpiperazin-1-yl)ethyl]-9-fluoro-2-(2-isopropyl-5-methyl-1,2,4-triazol-3-yl)-5,6-dihydroimidazo[1,2-d][1,4]benzoxazepine

HRID 1530732
ノート
印刷プレビュー

反応式

HRID 1530732 の反応式
Br[CH:2]([C:4]1[C:5]([F:27])=[CH:6][C:7]2[O:16][CH2:15][CH2:14][N:13]3[C:9](=[N:10][C:11]([C:17]4[N:18]([CH:23]([CH3:25])[CH3:24])[N:19]=[C:20]([CH3:22])[N:21]=4)=[CH:12]3)[C:8]=2[CH:26]=1)[CH3:3].[CH2:28]([N:30]1[CH2:35][CH2:34][NH:33][CH2:32][CH2:31]1)[CH3:29].CCN(C(C)C)C(C)C>O1CCOCC1>[CH2:28]([N:30]1[CH2:35][CH2:34][N:33]([CH:2]([C:4]2[C:5]([F:27])=[CH:6][C:7]3[O:16][CH2:15][CH2:14][N:13]4[CH:12]=[C:11]([C:17]5[N:18]([CH:23]([CH3:25])[CH3:24])[N:19]=[C:20]([CH3:22])[N:21]=5)[N:10]=[C:9]4[C:8]=3[CH:26]=2)[CH3:3])[CH2:32][CH2:31]1)[CH3:29]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 791961-EthylpiperazineHCID 81531DiisopropylethylamineHCID 683131309-(1-bromoethyl)-8-fluoro-2-(2-isopropyl-5-methyl-2H-[1,2,4]triazol-3-yl)-4,5-dihydro-6-oxa-1,3a-diazabenzo[e]azulene

生成物 1

HCID 6831291510-[1-(4-Ethylpiperazin-1-yl)ethyl]-9-fluoro-2-(2-isopropyl-5-methyl-1,2,4-triazol-3-yl)-5,6-dihydroimidazo[1,2-d][1,4]benzoxazepine収率 65%

試薬・触媒・溶媒 1

HCID 31275
1,4-Dioxane
溶媒

実験手順

A solution of 9-(1-bromoethyl)-8-fluoro-2-(2-isopropyl-5-methyl-2H-[1,2,4]triazol-3-yl)-4,5-dihydro-6-oxa-1,3a-diazabenzo[e]azulene (85 mg, 0.20 mmol), N-ethylpiperazine (27 μL, 0.22 mmol) and DIPEA (54 μL, 0.30 mmol) in dioxane (2 mL) was stirred at RT for 24 h. The reaction mixture was concentrated in vacuo and the residue was purified by column chromatography (Si-PPC, gradient 0-10% 2 M NH3/MeOH in DCM) to give 374 (61 mg, 0.13 mmol, 65% over 2 steps) as a white solid. LCMS (Method K): RT 2.74 min [M+H]+ 468.2. 1H NMR (CD3OD, 400 MHz): δ 8.55 (1H, d, J=8.2 Hz), 7.68 (1H, s), 6.76 (1H, d, J=11.1 Hz), 5.83 (1H, sept., J=6.7 Hz), 4.48 (4H, br s), 3.84 (1H, q, J=6.8 Hz), 2.50 (8H, br s), 2.38 (2H, q, J=7.4 Hz), 2.33 (3H, s), 1.53 (3H, d, J=6.7 Hz), 1.52 (3H, d, J=6.7 Hz), 1.40 (3H, d, J=6.8 Hz), 1.03 (3H, t, J=7.4 Hz)

後処理

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. customthe residue was purified by column chromatography (Si-PPC, gradient 0-10% 2 M NH3/MeOH in DCM)

出典と根拠

ORDレコード
ord-894c97e7a923409a99fe5bbb27e685f3
出典データセット
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09090628B2

反応ノート

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