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Trifluoroacetic acid → HCID 178507614、化合物

HRID 1486572
ノート
印刷プレビュー

反応式

HRID 1486572 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([NH:9][C:10]2[N:14]=[C:13]([NH:15][CH2:16][C:17]3[CH:18]=[CH:19][C:20]([NH:23]C(=O)OC(C)(C)C)=[N:21][CH:22]=3)[NH:12][N:11]=2)[CH:5]=[C:6]([Cl:8])[CH:7]=1.C(O)(C(F)(F)F)=O>C(Cl)Cl>[NH2:23][C:20]1[N:21]=[CH:22][C:17]([CH2:16][NH:15][C:13]2[NH:12][N:11]=[C:10]([NH:9][C:4]3[CH:3]=[C:2]([Cl:1])[CH:7]=[C:6]([Cl:8])[CH:5]=3)[N:14]=2)=[CH:18][CH: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

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 178452735HCID 178452735、化合物

生成物 1

HCID 178507614HCID 178507614、化合物収率 26%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of tert-butyl 5-((3-(3,5-dichlorophenylamino)-1H-1,2,4-triazol-5-ylamino)methyl)pyridin-2-ylcarbamate Compound 6 (50 mg, 111 μmol) in DCM (1 ml) was added TFA (1 ml) and the reaction was stirred for 1 hour. The reaction mixture was concentrated in vacuo and was partitioned between DCM (5 ml) and sat. NaHCO3 (3 ml). The layers were separated and the aqueous layer was extracted with DCM (3×5 ml). The combined organic solution was washed with brine (5 ml), dried over Na2SO4, filtered and concentrated to give a white solid as desired product (10.2 mg, 26% yield). MS +m/z: 350 (M+H)+

後処理

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. customwas partitioned between DCM (5 ml) and sat. NaHCO3 (3 ml)
  3. customThe layers were separated
  4. extractionthe aqueous layer was extracted with DCM (3×5 ml)
  5. washThe combined organic solution was washed with brine (5 ml)
  6. dry with materialdried over Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated

出典と根拠

ORDレコード
ord-bfe4b5383eb84c078df07037d31f1788
出典データセット
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09428469B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート