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Water → Methyl 4-amino-3-chloro-6-(7-fluoro-2-phenyl-1,3-benzoxazol-6-yl)pyridine-2-carboxylate

HRID 708932
ノート
印刷プレビュー

反応式

HRID 708932 の反応式
[NH2:1][C:2]1[CH:7]=[C:6](Br)[N:5]=[C:4]([C:9]([O:11][CH3:12])=[O:10])[C:3]=1[Cl:13].[F:14][C:15]1[C:23]2[O:22][C:21]([C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=3)=[N:20][C:19]=2[CH:18]=[CH:17][C:16]=1B(O)O.C([O-])([O-])=O.[K+].[K+].O>O1CCOCC1.Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1>[NH2:1][C:2]1[CH:7]=[C:6]([C:16]2[CH:17]=[CH:18][C:19]3[N:20]=[C:21]([C:24]4[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=4)[O:22][C:23]=3[C:15]=2[F:14])[N:5]=[C:4]([C:9]([O:11][CH3:12])=[O:10])[C:3]=1[Cl:13]
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 4

HCID 962Water2 回HCID 11430Potassium CarbonateHCID 22677536Methyl 4-amino-6-bromo-3-chloropicolinateHCID 71240109(7-Fluoro-2-phenyl-1,3-benzoxazol-6-yl)boronic acid

生成物 1

HCID 71239870Methyl 4-amino-3-chloro-6-(7-fluoro-2-phenyl-1,3-benzoxazol-6-yl)pyridine-2-carboxylate収率 36%

試薬・触媒・溶媒 2

HCID 178418476HCID 178418476、化合物触媒
HCID 312751,4-Dioxane溶媒

実験手順

0.024 g (0.03 mmol) of (PPh3)2PdCl2 is added to a solution of 0.3 g (1.13 mmol) of methyl 4-amino-6-bromo-3-chloropyridine-2-carboxylate in 20 ml of dioxane, and this mixture is stirred at room temperature (RT) for 30 min. In succession, 0.35 g (1.35 mmol) of (7-fluoro-2-phenyl-1,3-benzoxazol-6-yl)boronic acid, 0.47 g (3.4 mmol) of K2CO3 and 2 g (111 mmol) of H2O are then added to this mixture, which is then stirred under reflux for 6 h. The mixture is allowed to stand at RT for a further 12 h and then added to 40 ml of H2O. This mixture is extracted repeatedly with CH2Cl2, and the combined organic phase is dried over Na2SO4 and then concentrated. Purification by chromatography on silica gel using the mobile phase heptane/ethyl acetate (3/7) gives 0.16 g (36%) of product. 1H-NMR (CDCl3): δ 8.30, 8.00, 7.55 (3m, 5H, C6H5), 7.60, 7.55 (2d, 2H, benzoxazole ring), 7.30 (s, 1H, pyridine) 4.85 (bs, 2H, NH2), 4.00 (S, 3H, COOCH3).

後処理

  1. stirringis then stirred
  2. temperatureunder reflux for 6 h
  3. waitto stand at RT for a further 12 h
  4. extractionThis mixture is extracted repeatedly with CH2Cl2
  5. dry with materialthe combined organic phase is dried over Na2SO4
  6. concentrationconcentrated
  7. customPurification by chromatography on silica gel using the mobile phase heptane/ethyl acetate (3/7)

出典と根拠

ORDレコード
ord-23dc1d51197d454ebbd2f67c0bd273fd
出典データセット
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09179676B2

反応ノート

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