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Acetic Acid → methyl 2-(5-hydroxy-1E,3E,-tridecandienyl)-delta-oxobenzenpentanoate

HRID 1073644
ノート
印刷プレビュー

反応式

HRID 1073644 の反応式
C(O)(=O)C.O.O1CCCC1.C1COCC1.[O:16]=[C:17]([C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][C:26]=1/[CH:31]=[CH:32]/[CH:33]=[CH:34]/[CH:35]([O:44]C1CCCCO1)[CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH3:43])[CH2:18][CH2:19][CH2:20][C:21]([O:23][CH3:24])=[O:22]>C1COCC1>[OH:44][CH:35]([CH2:36][CH2:37][CH2:38][CH2:39][CH2:40][CH2:41][CH2:42][CH3:43])/[CH:34]=[CH:33]/[CH:32]=[CH:31]/[C:26]1[CH:27]=[CH:28][CH:29]=[CH:30][C:25]=1[C:17](=[O:16])[CH2:18][CH2:19][CH2:20][C:21]([O:23][CH3:24])=[O:22]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 176Acetic AcidHCID 962WaterHCID 14582854methyl delta-oxo-2-[5-[(tetrahydro-2H-pyran-2-yl)oxyl]-1E,3E-tridecadienyl]benzenepentanoateHCID 22180045THF tetrahydrofurane

生成物 1

HCID 14798470methyl 2-(5-hydroxy-1E,3E,-tridecandienyl)-delta-oxobenzenpentanoate収率 60.9%

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒

実験手順

To 1 ml of a 3:1:1 solution of acetic acid, water, and tetrahydrofuran THF) was added 20mg (0.041 mmol) of the titled product of Example 10 and the reaction mixture was allowed to stir 16 hr. After this time, some insoluble oil was still present and approximately 50μl of THF was added to the reaction mixture and it was stirred for an additional 2 hours. The volatile components were removed in vacuo and the residue was flash chromatographed. Elution with 1:1 diethylether-hexane produced b 10 mg of the desired product.

後処理

  1. stirringwas stirred for an additional 2 hours
  2. customThe volatile components were removed in vacuo
  3. customchromatographed
  4. washElution with 1:1 diethylether-hexane

出典と根拠

ORDレコード
ord-0db8553fa8ee49129d4aca936b19c16f
出典データセット
uspto-grants-1990_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04970234

反応ノート

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