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Pentaerythritol → 2,2-Bis(hydroxymethyl)propane-1,3-diyl dibutyrate

HRID 2258548
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HRID 2258548 반응식
[C:1]([O:6][CH2:7][C:8]([CH2:23][OH:24])([CH2:16][O:17][C:18](=[O:22])[CH2:19][CH2:20][CH3:21])[CH2:9][O:10][C:11](=[O:15])[CH2:12][CH2:13][CH3:14])(=[O:5])[CH2:2][CH2:3][CH3:4].OCC(CO)(CO)CO.[C:34](Cl)(=[O:38])[CH2:35][CH2:36][CH3:37]>N1C=CC=CC=1>[C:1]([O:6][CH2:7][C:8]([CH2:23][OH:24])([CH2:16][OH:17])[CH2:9][O:10][C:11](=[O:15])[CH2:12][CH2:13][CH3:14])(=[O:5])[CH2:2][CH2:3][CH3:4].[C:11]([O:10][CH2:9][C:8]([CH2:23][O:24][C:34](=[O:38])[CH2:35][CH2:36][CH3:37])([CH2:16][O:17][C:18](=[O:22])[CH2:19][CH2:20][CH3:21])[CH2:7][O:6][C:1](=[O:5])[CH2:2][CH2:3][CH3:4])(=[O:15])[CH2:12][CH2:13][CH3:14]
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참가 물질

6

반응물 3

HCID 8285Pentaerythritol3회HCID 8855Butyryl chloride2회HCID 22922626HCID 22922626, 화합물

생성물 2

HCID 81725Butanoic acid, 1,1'-(2,2-bis((1-oxobutoxy)methyl)-1,3-propanediyl) ester수율 14%HCID 441535362,2-Bis(hydroxymethyl)propane-1,3-diyl dibutyrate수율 26%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

In this example, pentaerythritol tributyrate, the tributyl ester of pentaerythritol, was synthesized from pentaerythritol and butyryl chloride as follows. To a solution of pentaerythritol (0.99 g, 7.28mmol) in dry pyridine (50 mL, under argon) at 0° C. was added butyryl chloride (2.3 mL, 22 mmol, 3 equiv) dropwise over one hour. The ice bath was removed after one hour, and the reaction stirred 24 hours at room temperature. Water (7 mL) was added and the bulk of pyridine was removed on the rotary evaporator at 2 Torr. The residue was dissolved in 1N HCL (12 mL) and the pentaerythritol esters extracted with CHCl3 (3×20 mL). The combined organic extracts were dried (MGSO4) and concentrated under vacuum to an oil (2.73 g). Purification by flash column chromatography using silica gel afforded the desired triester pentaerythritol tributyrate (1.34 g; 53%) as well as pentaerythritol dibutyrate (0.51 g; 26%) and pentaerythritol tetrabutyrate (0.42 g; 14%).

후처리

  1. customThe ice bath was removed after one hour
  2. additionWater (7 mL) was added
  3. customthe bulk of pyridine was removed on the rotary evaporator at 2 Torr
  4. dissolutionThe residue was dissolved in 1N HCL (12 mL)
  5. extractionthe pentaerythritol esters extracted with CHCl3 (3×20 mL)
  6. customThe combined organic extracts were dried (MGSO4)
  7. concentrationconcentrated under vacuum to an oil (2.73 g)
  8. customPurification by flash column chromatography

출처 및 근거

ORD 기록
ord-a10b2e22bc6a4c90985b4b9230e1439c
출처 데이터셋
uspto-grants-1997_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05661181

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