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N-Propyl-Methyl Piperidinium Bis(trifluoroMethylsulfonyl)Imide → (S)-ethyl 2-tert-butoxy-2-(7-(4-chlorophenyl)-5-methyl-2-(2-(1-(trifluoromethyl)-1H-indazol-5-yl)pyridin-4-yl)benzo[d]thiazol-6-yl)acetate

HRID 879351
ノート
印刷プレビュー

反応式

HRID 879351 の反応式
[NH:1]1[C:9]2[C:4](=[CH:5][C:6]([C:10]3[CH:15]=[C:14]([C:16]4[S:17][C:18]5[C:24]([C:25]6[CH:30]=[CH:29][C:28]([Cl:31])=[CH:27][CH:26]=6)=[C:23]([C@H:32]([O:38][C:39]([CH3:42])([CH3:41])[CH3:40])[C:33]([O:35][CH2:36][CH3:37])=[O:34])[C:22]([CH3:43])=[CH:21][C:19]=5[N:20]=4)[CH:13]=[CH:12][N:11]=3)=[CH:7][CH:8]=2)[CH:3]=[N:2]1.[F:44][C:45]([F:58])([F:57])I1C2C=CC=CC=2C(C)(C)O1.[N-](S(C(F)(F)F)(=O)=O)S(C(F)(F)F)(=O)=O>C(=S)=S>[C:39]([O:38][C@@H:32]([C:23]1[C:22]([CH3:43])=[CH:21][C:19]2[N:20]=[C:16]([C:14]3[CH:13]=[CH:12][N:11]=[C:10]([C:6]4[CH:5]=[C:4]5[C:9](=[CH:8][CH:7]=4)[N:1]([C:45]([F:58])([F:57])[F:44])[N:2]=[CH:3]5)[CH:15]=3)[S:17][C:18]=2[C:24]=1[C:25]1[CH:26]=[CH:27][C:28]([Cl:31])=[CH:29][CH:30]=1)[C:33]([O:35][CH2:36][CH3:37])=[O:34])([CH3:42])([CH3:41])[CH3:40]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 4176748N-Propyl-Methyl Piperidinium Bis(trifluoroMethylsulfonyl)ImideHCID 160435723,3-Dimethyl-1-(trifluoromethyl)-1,2-benziodoxoleHCID 86700148(S)-ethyl 2-(2-(2-(1H-indazol-5-yl)pyridin-4-yl)-7-(4-chlorophenyl)-5-methylbenzo[d]thiazol-6-yl)-2-tert-butoxyacetate

生成物 1

HCID 86700151(S)-ethyl 2-tert-butoxy-2-(7-(4-chlorophenyl)-5-methyl-2-(2-(1-(trifluoromethyl)-1H-indazol-5-yl)pyridin-4-yl)benzo[d]thiazol-6-yl)acetate

試薬・触媒・溶媒 1

HCID 6348Carbon Disulfide溶媒

実験手順

To a solution of (S)-ethyl 2-(2-(2-(1H-indazol-5-yl)pyridin-4-yl)-7-(4-chlorophenyl)-5-methylbenzo[d]thiazol-6-yl)-2-tert-butoxyacetate (40 mg, 0.065 mmol) in CS2 (1.5 mL), was added 1-Trifluoromethyl-3,3-dimethyl-1,2-benziodoxole (64 mg, 0.195 mmol), bis(trifluoromethane)sulfonimide (27 mg, 0.0975 mmol). The reaction mixture was heated at 60° C. in sealed microwave vial for 1d. The reaction mixture was washed by saturated NaHCO3, extracted by EtOAc, the organic phase was dried over MgSO4, filtered, concentrated down, purified by silica gel column, eluting by 0-50% EtOAc in hexanes to give the product. LCMS-ESI+: calc'd for C35H30ClF3N4O3S: 679.2 (M+H+); found: 679.2.

後処理

  1. washThe reaction mixture was washed by saturated NaHCO3
  2. extractionextracted by EtOAc
  3. dry with materialthe organic phase was dried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated down
  6. custompurified by silica gel column
  7. washeluting by 0-50% EtOAc in hexanes
  8. customto give the product

出典と根拠

ORDレコード
ord-290f9bc16bda4745ad44641c63c11cbe
出典データセット
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08987250B2

反応ノート

読み込み中…

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