Water → HCID 14204115、化合物

HRID 1722373ノート

反応式

HRID 1722373 の反応式
[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.[OH:16][CH2:17][CH2:18]CCCC12CC(=O)CC1CCC2.O>C(O)(=O)C>[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:16])[CH3:18]

参加物

5

反応物 3

HCID 962WaterHCID 14204106HCID 14204106、化合物HCID 20028720HCID 20028720、化合物

生成物 1

HCID 14204115HCID 14204115、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
75 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-71ff3e66a9064a25ae0380a87a98dd39
出典データセット
uspto-grants-1989_08
特許番号
US04855322

反応ノート

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