Acetic Acid → HCID 14204115, 화합물

HRID 1789550노트

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HRID 1789550 반응식
[OH:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH:7]1[CH2:14][CH2:13][CH:12]2[CH:8]1[CH2:9][C:10](=[O:15])[CH2:11]2.O.[C:17](O)(=[O:19])[CH3:18]>>[C:17]([O:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH:7]1[CH2:14][CH2:13][CH:12]2[CH:8]1[CH2:9][C:10](=[O:15])[CH2:11]2)(=[O:19])[CH3:18]

참가 물질

4

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온도
75 °C

실험 절차

The starting material 2-(5-hydroxypent-1-yl)bicyclo[3.3.0]octan-7-one {hexahydro-4-(5-hydroxypentyl)-2(1H)-pentalenone} (0.8 g, 3.8 mmoles) is diluted with glacial acetic acid (7 ml). The reaction is stirred and heated in a 75° C. oil bath for 24 hours, after which time water (20 ml) is added and the reaction partitioned between ether. The ether layer is separated and the aqueous phase extracted again with ether (2×50 ml). The extracts and the organic phase are combined and neutralized with saturated sodium bicarbonate. The organic phase is dried over anhydrous magnesium sulfate and the remained solvent removed under vacuum leaving a pale yellow oil. The product is kugelrohred under reduced pressure leaving a clear, colorless oil (0.5 g, 2.0 mmoles).

후처리

  1. customthe reaction partitioned between ether
  2. customThe ether layer is separated
  3. extractionthe aqueous phase extracted again with ether (2×50 ml)
  4. dry with materialThe organic phase is dried over anhydrous magnesium sulfate
  5. customthe remained solvent removed under vacuum
  6. customleaving a pale yellow oil

출처 및 근거

ORD 기록
ord-a562188c5ed14659b721a63cea1485be
출처 데이터셋
uspto-grants-1987_08
특허 번호
US04689345

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