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Trifluoroacetic acid → HCID 131732971, 화합물

HRID 2173434
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HRID 2173434 반응식
[OH:1][C@H:2]([C:18]1[CH:27]=[CH:26][C:21]2[C:22](=[O:25])[O:23][CH2:24][C:20]=2[C:19]=1[CH3:28])[CH2:3][N:4]1[CH:10]2[CH:8]([CH2:9]2)[N:7](C(OC(C)(C)C)=O)[CH2:6][CH2:5]1.[C:29]([OH:35])([C:31]([F:34])([F:33])[F:32])=[O:30]>C(Cl)Cl>[OH:35][C:29]([C:31]([F:34])([F:33])[F:32])=[O:30].[CH:10]12[CH2:9][CH:8]1[NH:7][CH2:6][CH2:5][N:4]2[CH2:3][C@@H:2]([C:18]1[CH:27]=[CH:26][C:21]2[C:22](=[O:25])[O:23][CH2:24][C:20]=2[C:19]=1[CH3:28])[OH:1]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 131732970HCID 131732970, 화합물

생성물 1

HCID 131732971HCID 131732971, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

In a round bottom flask charged with stirring bar, tert-butyl (±)5-[(2R)-2-hydroxy-2-(4-methyl-1-oxo-1,3-dihydro-2-benzofuran-5-yl)ethyl]-2,5-diazabicyclo[4.1.0]heptane-2-carboxylate (502 mg, 1.292 mmol) was dissolved in DCM (5 mL) and was treated with TFA (2 mL, 26.0 mmol) at room temperature for 3 hours. Then solvent was removed on rotavapor. Residue was re-dissolved in small amount of DCM and evaporated to take out remained TFA. Then it was dried on high vacuum pump for 4 hours to remove extra TFA. Without further purification, crude product was used to make ROMK inhibitors. LC/MS: (M+1)+=289.

후처리

  1. additionIn a round bottom flask charged
  2. customThen solvent was removed on rotavapor
  3. dissolutionResidue was re-dissolved in small amount of DCM
  4. customevaporated
  5. customThen it was dried on high vacuum pump for 4 hours
  6. customto remove extra TFA
  7. customWithout further purification, crude product

출처 및 근거

ORD 기록
ord-ee8cba956cab4ef681155ce5d05d7f7d
출처 데이터셋
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09056859B2

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