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HCID 20688053, 화합물 → HCID 59968773, 화합물

HRID 1596817
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HRID 1596817 반응식
[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]
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참가 물질

4

반응물 1

HCID 20688053HCID 20688053, 화합물

생성물 1

HCID 59968773HCID 59968773, 화합물수율 99.6%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 1049Pyridine용매

실험 절차

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

후처리

  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

출처 및 근거

ORD 기록
ord-549ba0a8bf9c4340b7eec59d4f6bf130
출처 데이터셋
uspto-grants-2001_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06291713B1

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