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Triethylamine → 2-[5-Bromo-3-(trifluoromethyl)-1h-pyrazol-1-yl]-1-[4-[4-(4,5-dihydro-5-phenyl-3-isoxazolyl)-2-thiazolyl]-1-piperidinyl]ethanone

HRID 2096018
ノート
印刷プレビュー

反応式

HRID 2096018 の反応式
[Br:1][C:2]1[N:6]([CH2:7][C:8]([OH:10])=O)[N:5]=[C:4]([C:11]([F:14])([F:13])[F:12])[CH:3]=1.C(Cl)(=O)C(Cl)=O.ClC1N(CC([N:30]2[CH2:35][CH2:34][CH:33]([C:36]3[S:37][CH:38]=[C:39]([C:41]4[CH2:45][CH:44]([C:46]5[CH:51]=[CH:50][CH:49]=[CH:48][CH:47]=5)[O:43][N:42]=4)[N:40]=3)[CH2:32][CH2:31]2)=O)N=C(C(F)(F)F)C=1.C(N(CC)CC)C>ClCCl.CN(C)C=O>[Br:1][C:2]1[N:6]([CH2:7][C:8]([N:30]2[CH2:35][CH2:34][CH:33]([C:36]3[S:37][CH:38]=[C:39]([C:41]4[CH2:45][CH:44]([C:46]5[CH:51]=[CH:50][CH:49]=[CH:48][CH:47]=5)[O:43][N:42]=4)[N:40]=3)[CH2:32][CH2:31]2)=[O:10])[N:5]=[C:4]([C:11]([F:14])([F:13])[F:12])[CH:3]=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 4

HCID 8471TriethylamineHCID 65578Oxalyl chlorideHCID 687439092-[5-chloro-3-(trifluoromethyl)-1H-pyrazol-1-yl]-1-[4-[4-(4,5-dihydro-5-phenyl-3-isoxazolyl)-2-thiazolyl]-1-piperidinyl]ethanoneHCID 687457105-bromo-3-(trifluoromethyl)-1H-pyrazole-1-acetic acid2 回

生成物 1

HCID 68743847
2-[5-Bromo-3-(trifluoromethyl)-1h-pyrazol-1-yl]-1-[4-[4-(4,5-dihydro-5-phenyl-3-isoxazolyl)-2-thiazolyl]-1-piperidinyl]ethanone

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide触媒HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of 5-bromo-3-(trifluoromethyl)-1H-pyrazole-1-acetic acid (i.e. the product of Example 11, Step D) (0.12 g, 0.61 mmol) in dichloromethane (5 mL) was added N,N-dimethylformamide (1 drop) followed by oxalyl chloride (0.25 mL, 2.86 mmol). The reaction mixture was stirred at room temperature for 1 h and then concentrated under reduced pressure. The residue containing crude acid chloride was taken up in dichloromethane (5 mL), and the solution was added dropwise to a mixture of 4-[4-(4,5-dihydro-5-phenyl-3-isoxazolyl)-2-thiazolyl]-1-piperidine hydrochloride (i.e. the intermediate of Example 10, Step F) (0.15 g, 0.43 mmol) and triethylamine (0.25 mL, 1.8 mmol) in dichloromethane (5 mL) at 0° C. The reaction mixture was allowed to warm to room temperature and then stirred overnight at room temperature. The mixture was then partitioned between 1.0 N aqueous hydrochloric acid solution and dichloromethane. The organic layer was washed with water, dried (MgSO4), concentrated under reduced pressure, and purified by medium-pressure liquid chromatography using ethyl acetate in hexanes as eluant to give 90 mg of the title product as an amorphous solid.

後処理

  1. concentrationconcentrated under reduced pressure
  2. additionThe residue containing crude acid chloride
  3. temperatureto warm to room temperature
  4. stirringstirred overnight at room temperature
  5. customThe mixture was then partitioned between 1.0 N aqueous hydrochloric acid solution and dichloromethane
  6. washThe organic layer was washed with water
  7. dry with materialdried (MgSO4)
  8. concentrationconcentrated under reduced pressure
  9. custompurified by medium-pressure liquid chromatography

出典と根拠

ORDレコード
ord-3144d2aa8a1b4235a9f9aae51e5d79df
出典データセット
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08449898B2

反応ノート

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