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Hydrochloric Acid → 7-[2,3-Dihydroxy-5-(3-hydroxyoct-1-enyl)cyclopentyl]heptanoic acid

HRID 372136
ノート
印刷プレビュー

反応式

HRID 372136 の反応式
[OH:1][CH:2]1[CH:6]([O:7]C2CCCCO2)[CH2:5][CH:4]([CH:14]=[CH:15][CH:16]([OH:22])[CH2:17][CH2:18][CH2:19][CH2:20][CH3:21])[CH:3]1[CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][C:29]([OH:31])=[O:30].Cl>C(O)C>[OH:1][CH:2]1[CH:6]([OH:7])[CH2:5][CH:4]([CH:14]=[CH:15][CH:16]([OH:22])[CH2:17][CH2:18][CH2:19][CH2:20][CH3:21])[CH:3]1[CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][C:29]([OH:31])=[O:30]
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 2

HCID 313Hydrochloric AcidHCID 543618807-[2-Hydroxy-5-(3-hydroxyoct-1-enyl)-3-(2-tetrahydropyranyloxy)cyclopentyl]heptanoic acid

生成物 1

HCID 542209287-[2,3-Dihydroxy-5-(3-hydroxyoct-1-enyl)cyclopentyl]heptanoic acid収率 3.6%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 7-[2-hydroxy-5-(3-hydroxyoct-1enyl)-3-(2-tetrahydropyranyloxy)cyclopentyl]heptanoic acid [0.34 g.; prepared as described above in Example 2(h)], ethanol (10 ml.), N aqueous hydrochloric acid (10 ml.) and a cation exchange resin [Dowex resin AG50W-X 8H+ (1.0 g.)] was stirred at 60°-62° C. for 8 hours. The mixture was filtered and the solid was washed with ethanol. The combined filtrate and washings were concentrated in vacuo to remove most of the ethanol, and the residue was extracted twice with diethyl ether. The combined ethereal extracts were extracted with 2N aqueous sodium carbonate solution, and the aqueous extract was acidified to pH 1 by the addition of concentrated hydrochloric acid. The resulting aqueous mixture was extracted with diethyl ether and the ethereal extract was dried over magnesium sulphate and evaporated to dryness. The residue (0.13 g.) was subjected to preparative thin-layer chromatography on silica gel, using a mixture of ethyl acetate, cyclohexane and formic acid (40:40:1 by volume) as the eluent, to give 7-[2,3-dihydroxy-5-(3-hydroxyoct-1-enyl)cyclopentyl]heptanoic acid (0.01 g.), νmax 1700 cm-1, 980 cm-1. Elemental analysis: found: C, 67.8; H, 10.4%; C20H36O5 requires C, 67.4; H, 10.2%.

後処理

  1. filtrationThe mixture was filtered
  2. washthe solid was washed with ethanol
  3. concentrationThe combined filtrate and washings were concentrated in vacuo
  4. customto remove most of the ethanol
  5. extractionthe residue was extracted twice with diethyl ether
  6. extractionThe combined ethereal extracts were extracted with 2N aqueous sodium carbonate solution
  7. extractionthe aqueous extract
  8. additionwas acidified to pH 1 by the addition of concentrated hydrochloric acid
  9. extractionThe resulting aqueous mixture was extracted with diethyl ether
  10. extractionthe ethereal extract
  11. dry with materialwas dried over magnesium sulphate
  12. customevaporated to dryness
  13. additiona mixture of ethyl acetate, cyclohexane and formic acid (40:40:1 by volume) as the eluent

出典と根拠

ORDレコード
ord-7b4cff3be016492880d8a0848e561946
出典データセット
uspto-grants-1978_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04088821

反応ノート

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