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Trifluoroacetic acid → HCID 69933247、化合物

HRID 540797
ノート
印刷プレビュー

反応式

HRID 540797 の反応式
[F:1][C:2]([F:40])([F:39])[C:3]1[CH:38]=[CH:37][C:6]([O:7][C:8]2[N:12]([CH2:13][C:14]([N:16]([CH3:18])[CH3:17])=[O:15])[N:11]=[C:10]([C:19]3[CH:20]=[C:21]([C:25]4([NH:29]C(=O)OC(C)(C)C)[CH2:28][O:27][CH2:26]4)[CH:22]=[CH:23][CH:24]=3)[CH:9]=2)=[CH:5][CH:4]=1.C(O)(C(F)(F)F)=O>C(Cl)Cl>[NH2:29][C:25]1([C:21]2[CH:20]=[C:19]([C:10]3[CH:9]=[C:8]([O:7][C:6]4[CH:5]=[CH:4][C:3]([C:2]([F:1])([F:39])[F:40])=[CH:38][CH:37]=4)[N:12]([CH2:13][C:14]([N:16]([CH3:18])[CH3:17])=[O:15])[N:11]=3)[CH:24]=[CH:23][CH:22]=2)[CH2:28][O:27][CH2:26]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 69932959HCID 69932959、化合物

生成物 1

HCID 69933247HCID 69933247、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A stirred solution of tert-butyl [3-(3-{5-(4-trifluoromethylphenoxy)-1-[2-(dimethylamino)-2-oxoethyl]-1H-pyrazol-3-yl}phenyl)oxetan-3-yl]carbamate (70 mg, 0.13 mmol) in 2 mL of CH2Cl2 was cooled in an ice bath. To the solution was added 1 mL of TFA and the mixture was stirred for 1 h. The cooling bath was removed and the mixture was stirred at ambient temperature for 1 h. 10% Aqueous Na2CO3 solution was added and the mixture was extracted with CH2Cl2. The combined organic phases were dried over Na2SO4, filtered, and the solvent was removed under reduced pressure to give 2-{3-[3-(3-aminooxetan-3-yl)phenyl]-5-(4-trifluoromethylphenoxy)-1H-pyrazol-1-yl}-N,N-dimethylacetamide as an oil. Calcd (M+1)+: 461.4. Found: 461.5

後処理

  1. customThe cooling bath was removed
  2. stirringthe mixture was stirred at ambient temperature for 1 h
  3. addition10% Aqueous Na2CO3 solution was added
  4. extractionthe mixture was extracted with CH2Cl2
  5. dry with materialThe combined organic phases were dried over Na2SO4
  6. filtrationfiltered
  7. customthe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-6c29bf2ee8734986b24e5f3af6db96b8
出典データセット
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08871796B2

反応ノート

読み込み中…

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