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Heptane → HCID 86665238、化合物

HRID 1028084
ノート
印刷プレビュー

反応式

HRID 1028084 の反応式
[OH-].[Na+].[CH2:3]([OH:23])[CH2:4][CH2:5][CH2:6]/[CH:7]=[CH:8]\[CH2:9]/[CH:10]=[CH:11]\[CH2:12]/[CH:13]=[CH:14]\[CH2:15]/[CH:16]=[CH:17]\[CH2:18]/[CH:19]=[CH:20]\[CH2:21][CH3:22].[C:24]([O:28][C:29](=[O:34])[CH:30](Br)[CH2:31]C)([CH3:27])([CH3:26])[CH3:25].[CH3:35][CH2:36]CCCCC>S(=O)(=O)(O)[O-].C([N+](CCCC)(CCCC)CCCC)CCC.C1(C)C=CC=CC=1>[CH2:3]([O:23][CH:30]([CH3:31])[C:29]([O:28][C:24]([CH3:25])([CH3:26])[CH3:27])=[O:34])[CH2:4][CH2:5]/[CH:6]=[CH:7]\[CH2:8]/[CH:9]=[CH:10]\[CH2:11]/[CH:12]=[CH:13]\[CH2:14]/[CH:15]=[CH:16]\[CH2:17]/[CH:18]=[CH:19]\[CH2:20]/[CH:21]=[CH:22]\[CH2:35][CH3:36]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 8900HeptaneHCID 14798Sodium HydroxideHCID 13124118tert-Butyl 2-bromobutanoate2 回HCID 59539494(5Z,8Z,11Z,14Z,17Z)-icosa-5,8,11,14,17-pentaen-1-ol

生成物 1

HCID 86665238HCID 86665238、化合物

試薬・触媒・溶媒 2

HCID 94433
Tetrabutylammonium hydrogen sulfate
触媒
HCID 1140Toluene溶媒

反応条件

温度
50 °C

実験手順

An aqueous solution of sodium hydroxide (50% (w/w), 6 ml) was added portionwise to a mixture of (5Z,8Z,11Z,14Z,17Z)-icosa-5,8,11,14,17-pentaen-1-ol (2.01 g, 6.39 mmol), tert-butyl-2-bromobutyrat (2.85 g, 12.8 mmol) and tetrabutylammonium bisulfate (0.65 g, 1.91 mmol) in toluene (12 ml). The reaction mixture was vigorously stirred under N2-atmosphere and warmed to 50° C. The reaction mixture was stirred at 50° C. for a total of 22 hrs. Additional tert-butyl-2-bromobutyrat (1.43 g, 6.39 mmol) and (1.44 g, 6.44 mmol) was added after 1½ hrs and 3 hrs respectively. The mixture was cooled and added ice-water (˜50 ml) and heptane (50 ml), the phases were separated and the organic phase was concentrated under reduced pressure. Flash chromatography on silica gel (30 g) eluting with heptane-heptane/EtOAc (99:1) yielded 2.12 g of the title compound as a liquid. 1H NMR (300 MHz, CDCl3) δ 0.94-1.04 (m, 6H), 1.47 (s, 9H), 1.68-1.85 (m, 4H), 1.93-2.20 (m, 4H), 2.80-2.86 (m, 10H), 3.28-3.36 (m, 1H), 3.55-3.63 (m, 2H), 5.27-5.43 (m, 12H)

後処理

  1. stirringThe reaction mixture was stirred at 50° C. for a total of 22 hrs
  2. temperatureThe mixture was cooled
  3. customthe phases were separated
  4. concentrationthe organic phase was concentrated under reduced pressure
  5. washFlash chromatography on silica gel (30 g) eluting with heptane-heptane/EtOAc (99:1)

出典と根拠

ORDレコード
ord-b3fcf8b52cd84787bd91e839da111cca
出典データセット
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08735436B2

反応ノート

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