HCID 21875489、化合物 → HCID 21875359、化合物

HRID 966912ノート

反応式

HRID 966912 の反応式
[N+:1]([C:4]1[C:13]2[N:12]=[CH:11][CH:10]=[N:9][C:8]=2[C:7]([C:14]#[N:15])=[CH:6][CH:5]=1)([O-])=O.[H][H]>C(OCC)(=O)C.C(O)C.[Pd]>[NH2:1][C:4]1[C:13]2[NH:12][CH2:11][CH2:10][NH:9][C:8]=2[C:7]([C:14]#[N:15])=[CH:6][CH:5]=1

参加物

6

反応物 2

HCID 21875489HCID 21875489、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 21875359HCID 21875359、化合物収率 92.5%

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 702Ethanol溶媒HCID 8857Ethyl Acetate溶媒

実験手順

Compound 468A (0.037 g, 0.18 mmol) was dissolved in a mixture of ethyl acetate (1.0 mL)/ethanol (1.0 mL) and 10% Pd/C (0.050 g) was added. Hydrogen was then introduced via a balloon. After 2 h, the reaction was purged with nitrogen and filtered through Celite, rinsing with ethyl acetate. Concentration in vacuo gave 0.029 g (90%) of compound 469A as a red oil, which was taken on without further purification. HPLC: 97% at 3.217 min (retention time) (YMC S5 ODS column, 4.6×50 mm, eluting with 10-90% aqueous methanol over 4 min containing 0.2% phosphoric acid, 4 mL/min, monitoring at 220 nm).

後処理

  1. additionwas added
  2. customthe reaction was purged with nitrogen
  3. filtrationfiltered through Celite
  4. washrinsing with ethyl acetate
  5. concentrationConcentration in vacuo

出典と根拠

ORDレコード
ord-ef46af3c1da54f1b96f8364bc4221604
出典データセット
uspto-grants-2005_10
特許番号
US06953679B2

反応ノート

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