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Potassium Carbonate → Methyl 2-[4-[4-hydroxy-1-[3-(trifluoromethyl)-[1,2,4]triazolo[4,3-b]pyridazin-6-yl]piperidin-4-yl]phenoxy]acetate

HRID 1675167
ノート
印刷プレビュー

反応式

HRID 1675167 の反応式
Br[CH2:2][C:3]([O:5][CH3:6])=[O:4].[OH:7][C:8]1[CH:13]=[CH:12][C:11]([C:14]2([OH:33])[CH2:19][CH2:18][N:17]([C:20]3[CH:21]=[CH:22][C:23]4[N:24]([C:26]([C:29]([F:32])([F:31])[F:30])=[N:27][N:28]=4)[N:25]=3)[CH2:16][CH2:15]2)=[CH:10][CH:9]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[OH:33][C:14]1([C:11]2[CH:10]=[CH:9][C:8]([O:7][CH2:2][C:3]([O:5][CH3:6])=[O:4])=[CH:13][CH:12]=2)[CH2:15][CH2:16][N:17]([C:20]2[CH:21]=[CH:22][C:23]3[N:24]([C:26]([C:29]([F:32])([F:31])[F:30])=[N:27][N:28]=3)[N:25]=2)[CH2:18][CH2:19]1
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 11430Potassium CarbonateHCID 60984Methyl bromoacetateHCID 667887034-(4-Hydroxyphenyl)-1-[3-(trifluoromethyl)[1,2,4]triazolo[4,3-b]pyridazin-6-yl]piperidin-4-ol

生成物 1

HCID 67340075Methyl 2-[4-[4-hydroxy-1-[3-(trifluoromethyl)-[1,2,4]triazolo[4,3-b]pyridazin-6-yl]piperidin-4-yl]phenoxy]acetate収率 100.1%

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

実験手順

Methyl 2-bromoacetate (0.121 mL, 1.28 mmol) was added to 4-(4-hydroxyphenyl)-1-[3-(trifluoromethyl)[1,2,4]triazolo[4,3-b]pyridazin-6-yl]piperidin-4-ol (323 mg, 0.85 mmol) and potassium carbonate (235 mg, 1.70 mmol) in DMF (5 mL). The resulting suspension was stirred at ambient temperature for 16 hours. The reaction mixture was evaporated to dryness, then water (50 mL) was added and the mixture was stirred for 20 minutes. The resulting precipitate was collected by filtration, washed with water then ether and dried to afford methyl 2-[4-[4-hydroxy-1-[3-(trifluoromethyl)-[1,2,4]triazolo[4,3-b]pyridazin-6-yl]piperidin-4-yl]phenoxy]acetate (384 mg, 100%) as a beige solid.

後処理

  1. customThe reaction mixture was evaporated to dryness
  2. additionwater (50 mL) was added
  3. stirringthe mixture was stirred for 20 minutes
  4. filtrationThe resulting precipitate was collected by filtration
  5. washwashed with water
  6. dry with materialether and dried

出典と根拠

ORDレコード
ord-972e1c9be7ab4ffea26d17dca33f1351
出典データセット
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08003649B2

反応ノート

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