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Diisopropylethylamine → HCID 25054678、化合物

HRID 1400089
ノート
印刷プレビュー

反応式

HRID 1400089 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([C:9]([F:12])([F:11])[F:10])[N:6]=[N:5][C:4]=1[NH:13][CH:14]1[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]1.[F:20][C:21]([F:31])([F:30])[C:22]1[CH:23]=[C:24]([CH:27]=[CH:28][CH:29]=1)[CH2:25]Br.C(N(C(C)C)CC)(C)C>C(#N)C.Cl.C(OCC)C>[CH3:1][O:2][C:3]1[CH:8]=[C:7]([C:9]([F:12])([F:10])[F:11])[N:6]=[N:5][C:4]=1[NH:13][CH:14]1[CH2:19][CH2:18][N:17]([CH2:25][C:24]2[CH:27]=[CH:28][CH:29]=[C:22]([C:21]([F:20])([F:30])[F:31])[CH:23]=2)[CH2:16][CH2:15]1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 81531DiisopropylethylamineHCID 1230611-(Bromomethyl)-3-(trifluoromethyl)benzeneHCID 59233384HCID 59233384、化合物

生成物 1

HCID 25054678HCID 25054678、化合物収率 109.6%

試薬・触媒・溶媒 3

HCID 313Hydrochloric Acid溶媒HCID 3283Diethyl Ether
溶媒
HCID 6342Acetonitrile溶媒

実験手順

A mixture of (4-methoxy-6-trifluoromethyl-pyridazin-3-yl)-piperidin-4-yl-amine (D8) (0.10 g, 0.36 mmol), 3-trifluoromethyl-benzyl bromide (0.060 ml, 0.29 mmol) and diisopropylethylamine (0.138 ml, 0.79 mmol) in acetonitrile (2 ml) was stirred at room temperature for 16 h. After this period, the solvent was evaporated in vacuo and the crude product purified by short open column chromatography (silica gel; 3% ammonia in methanol (7M)/dichloromethane). The desired fractions were collected and evaporated in vacuo. The product thus obtained was dissolved in a solution 2M of hydrochloric acid in diethyl ether to yield the corresponding hydrochloride salt E4 (0.138 g, 88%) as a solid. C19H20F6N4O.HCl free base requires 434; Found 435 (MH+). Rt (Method 1): 4.73 min.

後処理

  1. waitAfter this period
  2. customthe solvent was evaporated in vacuo
  3. customthe crude product purified by short open column chromatography (silica gel; 3% ammonia in methanol (7M)/dichloromethane)
  4. customThe desired fractions were collected
  5. customevaporated in vacuo
  6. customThe product thus obtained

出典と根拠

ORDレコード
ord-7c270af2c9c94b389ea2362407568e99
出典データセット
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08906921B2

反応ノート

読み込み中…

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