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Phosgene → 4-{4-[(2-Phenyl-5-trifluoromethyl-oxazole-4-carbonyl)-amino]-phenyl}-piperazine-1-carboxylic acid (3-methyl-pyridin-2-yl)-amide

HRID 1641845
ノート
印刷プレビュー

反応式

HRID 1641845 の反応式
[NH2:1][C:2]1[C:7]([CH3:8])=[CH:6][CH:5]=[CH:4][N:3]=1.C(N(CC)CC)C.[C:16](Cl)(Cl)=[O:17].C1COCC1.Cl.[N:26]1([C:32]2[CH:37]=[CH:36][C:35]([NH:38][C:39]([C:41]3[N:42]=[C:43]([C:50]4[CH:55]=[CH:54][CH:53]=[CH:52][CH:51]=4)[O:44][C:45]=3[C:46]([F:49])([F:48])[F:47])=[O:40])=[CH:34][CH:33]=2)[CH2:31][CH2:30][NH:29][CH2:28][CH2:27]1>C(Cl)Cl.CN1CCCC1=O.C(OCC)(=O)C>[CH3:8][C:7]1[C:2]([NH:1][C:16]([N:29]2[CH2:30][CH2:31][N:26]([C:32]3[CH:37]=[CH:36][C:35]([NH:38][C:39]([C:41]4[N:42]=[C:43]([C:50]5[CH:55]=[CH:54][CH:53]=[CH:52][CH:51]=5)[O:44][C:45]=4[C:46]([F:47])([F:49])[F:48])=[O:40])=[CH:34][CH:33]=3)[CH2:27][CH2:28]2)=[O:17])=[N:3][CH:4]=[CH:5][CH:6]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

9

反応物 5

HCID 6371PhosgeneHCID 8028TetrahydrofuranHCID 8471Triethylamine2 回HCID 153472-Amino-3-methylpyridineHCID 667383362-Phenyl-5-trifluoromethyl-oxazole-4-carboxylic acid (4-piperazin-1-yl-phenyl)-amide hydrochloride

生成物 1

HCID 57652030
4-{4-[(2-Phenyl-5-trifluoromethyl-oxazole-4-carbonyl)-amino]-phenyl}-piperazine-1-carboxylic acid (3-methyl-pyridin-2-yl)-amide
収率 16%

試薬・触媒・溶媒 3

HCID 6344Dichloromethane溶媒HCID 8857Ethyl Acetate溶媒HCID 13387N-methyl-2-pyrrolidone溶媒

反応条件

温度
-40 °C

実験手順

To a solution of 2-amino-3-picoline (26 μL, 0.204 mmol) and triethylamine (63 μL, 0.448 mmol) in 5 mL methylene chloride at −40° C. was slowly added a 20% solution of phosgene in THF (118 μL, 0.224 mmol). The reaction mixture was stirred at −40° C. for 1 hr and then a solution of 2-phenyl-5-trifluoromethyl-oxazole-4-carboxylic acid (4-piperazin-1-yl-phenyl)-amide hydrochloride (100 mg, 0.204 mmol) and triethylamine (57 μl, 0.408 mmol) in 8 ml of 1-methyl-2-pyrrolidinone was slowly added and stirred at room temperature overnight. The reaction mixture was diluted with ethyl acetate and washed with saturated sodium bicarbonate solution and water. The organic layer was dried over magnesium sulfate, filtered and evaporated to dryness. The residue was purified by flash chromatography (eluting with ethyl acetate/hexane) to yield 4-{4-[(2-phenyl-5-trifluoromethyl-oxazole-4-carbonyl)-amino]-phenyl}-piperazine-1-carboxylic acid (3-methyl-pyridin-2-yl)-amide (18 mg, 16%). ES-MS calcd for C28H25F3N6O3 (m/e) 550.6, obsd 551.1 (M+H).

後処理

  1. stirringstirred at room temperature overnight
  2. washwashed with saturated sodium bicarbonate solution and water
  3. dry with materialThe organic layer was dried over magnesium sulfate
  4. filtrationfiltered
  5. customevaporated to dryness
  6. customThe residue was purified by flash chromatography (eluting with ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-6fd4d8ce48fc4a2baf8ec61bff0856e7
出典データセット
uspto-grants-2012_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08115011B2

反応ノート

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