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HCID 20688053、化合物 → HCID 59968773、化合物

HRID 1596817
ノート
印刷プレビュー

反応式

HRID 1596817 の反応式
[C:1]([C:5]([OH:16])([CH2:10][C:11]#[C:12][CH2:13][CH2:14][CH3:15])[C:6]([CH3:9])([CH3:8])[CH3:7])([CH3:4])([CH3:3])[CH3:2]>N1C=CC=CC=1.[Pd]>[C:1]([C:5]([OH:16])([CH2:10]/[CH:11]=[CH:12]\[CH2:13][CH2:14][CH3:15])[C:6]([CH3:7])([CH3:8])[CH3:9])([CH3:3])([CH3:4])[CH3:2]
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 20688053HCID 20688053、化合物

生成物 1

HCID 59968773HCID 59968773、化合物収率 99.6%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 1049Pyridine溶媒

実験手順

50 mg of a catalyst of 5% palladium on barium sulfate were added at once to a stirred solution of 500 mg (2.23 mmol) 3-tert-butyl-2,2-dimethylnon-5-in-3-ol in 5 ml pyridine. The mixture obtained was degassed three times, exposed to a hydrogen atmosphere and stirred overnight. Subsequently, it was diluted with 100 ml pentane and filtered over silica gel. The silica gel was washed with 100 ml Et2O. The combined organic phases were washed with a copper sulfate solution (5×100 ml), with H2O (100 ml) and with salt solution (50 ml), dried and concentrated under reduced pressure. There were obtained 503 mg (99%) (Z)-3-tert-butyl-2,2-dimethylnon-5-en-3-ol

後処理

  1. customThe mixture obtained
  2. customwas degassed three times
  3. additionSubsequently, it was diluted with 100 ml pentane
  4. filtrationfiltered over silica gel
  5. washThe silica gel was washed with 100 ml Et2O
  6. washThe combined organic phases were washed with a copper sulfate solution (5×100 ml), with H2O (100 ml) and with salt solution (50 ml)
  7. customdried
  8. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-549ba0a8bf9c4340b7eec59d4f6bf130
出典データセット
uspto-grants-2001_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06291713B1

反応ノート

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