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HCID 67367246、化合物 → HCID 67367265、化合物

HRID 1895758
ノート
印刷プレビュー

反応式

HRID 1895758 の反応式
C([O:8][C:9]1[CH:14]=[CH:13][N:12]([C:15]2[CH:22]=[CH:21][C:18]([C:19]#[N:20])=[CH:17][C:16]=2[F:23])[C:11](=[O:24])[CH:10]=1)C1C=CC=CC=1>[Pd].CO>[F:23][C:16]1[CH:17]=[C:18]([CH:21]=[CH:22][C:15]=1[N:12]1[CH:13]=[CH:14][C:9]([OH:8])=[CH:10][C:11]1=[O:24])[C:19]#[N:20]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 67367246HCID 67367246、化合物

生成物 1

HCID 67367265HCID 67367265、化合物

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

To 4-(4-(benzyloxy)-2-oxopyridin-1(2H)-yl)-3-fluorobenzonitrile (250 mg, 0.780 mmol) and 10% palladium on carbon (50 mg, 0.470 mmol) was applied vacuum then placed under an atmosphere of nitrogen. Methanol (5 mL)was added and vacuum applied briefly. The reaction was placed under an atmosphere of hydrogen for 6 hours. The reaction mixture was passed through a 10×10 mm CELITE® 545 filter aid plug eluting with an additional 10 mL each of MeOH and CH2Cl2. The filtrate was concentrated to 170 mg of a pale tan foam. Added 5 mL MeOH and heated to reflux, filtered hot and rinsed with 3×2 mL warm MeOH. The filtrate was concentrated to crude product (166 mg, 0.577 mmol, 74%) as a pale yellow solid which was used as obtained in the subsequent step. MS (ESI) 231.1 (M+1).

後処理

  1. filtrationfilter aid plug
  2. washeluting with an additional 10 mL each of MeOH and CH2Cl2
  3. concentrationThe filtrate was concentrated to 170 mg of a pale tan foam
  4. additionAdded 5 mL MeOH
  5. temperatureheated
  6. temperatureto reflux
  7. filtrationfiltered hot
  8. washrinsed with 3×2 mL
  9. temperaturewarm MeOH
  10. customas obtained in the subsequent step

出典と根拠

ORDレコード
ord-f58b43a95a424f24b2cf5ed9e423c638
出典データセット
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08513424B2

反応ノート

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