Trifluoroacetic acid → HCID 67099670、化合物

HRID 1868725ノート

反応式

HRID 1868725 の反応式
[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]

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 67099651HCID 67099651、化合物

生成物 1

HCID 67099670HCID 67099670、化合物収率 38.9%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-73af7287e5ae48b9876cc321a98cfee0
出典データセット
uspto-grants-2009_12
特許番号
US07635715B2

反応ノート

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