Trifluoroacetic acid → HCID 67099670, 화합물

HRID 2078133노트

반응식

HRID 2078133 반응식
[C:1]([C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[C:9]([CH3:14])([CH3:13])[C:8](=[O:15])[C:7]([C:16]([NH:18][CH2:19][C:20]([O:22]C(C)(C)C)=[O:21])=[O:17])=[C:6]2[OH:27])#[N:2].C(O)(C(F)(F)F)=O>O>[C:1]([C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[C:9]([CH3:14])([CH3:13])[C:8](=[O:15])[C:7]([C:16]([NH:18][CH2:19][C:20]([OH:22])=[O:21])=[O:17])=[C:6]2[OH:27])#[N:2]

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 67099651HCID 67099651, 화합물

생성물 1

HCID 67099670HCID 67099670, 화합물수율 38.9%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

1,1-Dimethylethyl N-((6-cyano-4-hydroxy-1,1-dimethyl-2-oxo-naphthalene-3-yl)carbonyl)glycinate (124 mg, 335 μmol) was stirred in TFA (1 mL, 13462 μmol) at room temperature for 15 minutes. Water was added. The resulting precipitate was filtered. The green solid was dissolved in saturated NaHCO3 and washed with DCM. The aqueous layer was separated and acidified with 10% HCl. The resulting precipitate was filtered and washed with water to give the desired product as a white solid (41 mg). MS (m/e)=315.1 (M+H)+. Calculated for C16H14N2O5 314.09.

후처리

  1. filtrationThe resulting precipitate was filtered
  2. dissolutionThe green solid was dissolved in saturated NaHCO3
  3. washwashed with DCM
  4. customThe aqueous layer was separated
  5. filtrationThe resulting precipitate was filtered
  6. washwashed with water

출처 및 근거

ORD 기록
ord-f38ae4f850814a298a98657d8a38b9f5
출처 데이터셋
uspto-grants-2011_04
특허 번호
US07928139B2

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