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Trifluoroacetic acid → HCID 46199246、化合物

HRID 1959348
ノート
印刷プレビュー

反応式

HRID 1959348 の反応式
C(OC([N:8](C(OC(C)(C)C)=O)[C:9]1[C:10]([C:16]2[N:20](C(OC(C)(C)C)=O)[C:19]3[CH:28]=[C:29]([CH3:32])[CH:30]=[CH:31][C:18]=3[N:17]=2)=[N:11][C:12](Br)=[CH:13][N:14]=1)=O)(C)(C)C.[NH:40]1[CH2:45][CH2:44]S[CH2:42][CH2:41]1.C1C=C(Cl)C=C(C(OO)=O)C=1.C(O)(C(F)(F)F)=O.C([O-])([O-])=O.[Na+].[Na+].[O-:70][S:71]([O-:74])(=S)=O.[Na+].[Na+]>CN(C=O)C.CCOC(C)=O>[O:70]=[S:71]1(=[O:74])[CH2:44][CH2:45][N:40]([C:12]2[N:11]=[C:10]([C:16]3[NH:20][C:19]4[CH:28]=[C:29]([CH3:32])[CH:30]=[CH:31][C:18]=4[N:17]=3)[C:9]([NH2:8])=[N:14][CH:13]=2)[CH2:41][CH2:42]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 6422Trifluoroacetic acidHCID 67164ThiomorpholineHCID 70297m-Chloroperbenzoic acidHCID 20482104HCID 20482104、化合物HCID 86661948HCID 86661948、化合物

生成物 1

HCID 46199246HCID 46199246、化合物収率 31%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
60 °C

実験手順

A solution of tert-butyl 2-[3-[bis(tert-butoxycarbonyl)amino]-6-bromo-pyrazin-2-yl]-6-methyl-benzimidazole-1-carboxylate (70 mg, 0.1158 mmol) in DMF (2 mL) was treated with thiomorpholine (59.74 mg, 0.5790 mmol) and heated to 60° C. for 3 hours. The mixture was then diluted with EtOAc, washed with water, brine, dried (MgSO4) and concentrated in vacuo. The residue was dissolved in DCM (10 mL), treated with mCPBA (59.95 mg, 0.3474 mmol) and stirred at RT for 1 hour. After washing with a 1:1 Na2CO3/Na2S2O3 solution, TFA (264.1 mg, 178.4 μL, 2.316 mmol) was added and the mixture stirred at RT for 1 hour. This was concentrated in vacuo and the resultant residue was purified by reverse phase preparative HPLC [Waters Sunfire C18, 10 uM, 100A column, gradient 10%-95% B (solvent A: 0.05% TFA in water, solvent B: CH3CN) over 16 minutes at 25 mL/min]. The fractions were collected and freeze-dried to give the title compound (13.1 mg, 31% Yield).

後処理

  1. washwashed with water, brine
  2. dry with materialdried (MgSO4)
  3. concentrationconcentrated in vacuo
  4. dissolutionThe residue was dissolved in DCM (10 mL)
  5. additionwas added
  6. stirringthe mixture stirred at RT for 1 hour
  7. concentrationThis was concentrated in vacuo
  8. customthe resultant residue was purified by reverse phase preparative HPLC [Waters Sunfire C18, 10 uM, 100A column, gradient 10%-95% B (solvent A: 0.05% TFA in water, solvent B: CH3CN) over 16 minutes at 25 mL/min]
  9. customThe fractions were collected
  10. customfreeze-dried

出典と根拠

ORDレコード
ord-c62c62b36c5c479d86d1642890072497
出典データセット
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08410112B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート