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Pentaerythritol → HCID 22922627、化合物

HRID 2258550
ノート
印刷プレビュー

反応式

HRID 2258550 の反応式
OC[C:3]([CH2:8][OH:9])([CH2:6]O)CO.[C:10]([O:15][CH2:16][C:17]([CH2:27][OH:28])([CH2:25][OH:26])[CH2:18][O:19][C:20](=[O:24])[CH2:21][CH2:22][CH3:23])(=[O:14])[CH2:11][CH2:12][CH3:13].[C:29](Cl)(=[O:32])[CH2:30][CH3:31]>N1C=CC=CC=1>[C:29]([O:26][CH2:25][C:17]([CH2:27][O:28][C:8](=[O:9])[CH2:3][CH3:6])([CH2:18][O:19][C:20](=[O:24])[CH2:21][CH2:22][CH3:23])[CH2:16][O:15][C:10](=[O:14])[CH2:11][CH2:12][CH3:13])(=[O:32])[CH2:30][CH3:31]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8285PentaerythritolHCID 62324Propionyl chlorideHCID 441535362,2-Bis(hydroxymethyl)propane-1,3-diyl dibutyrate2 回

生成物 1

HCID 22922627HCID 22922627、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

In this example, pentaerythritol dibutyratedipropionate was prepared from pentaerythritol dibutyrate as follows. To a solution of pentaerythritol dibutyrate (0.5 g; 1.81 mmol) in dry pyridine (10 mL, under argon) at 0° C. was added propionyl chloride (0.6 mL) dropwise over one hour. The ice bath was removed after one hour, and the reaction stirred 24 hours at room temperature. Water (5 mL) was added and the bulk of pyridine was removed on the rotary evaporator at 2 Torr. The residue was dissolved in 1N HCL (5 mL) and the desired product extracted with CHCl3 (2×20 mL). The combined organic extracts were dried (MgSO4) and concentrated under vacuum. Purification of the crude product by flash column chromatography using silica gel afforded pentaerythritol dibutyrate dipropionate (0.6 g).

後処理

  1. customThe ice bath was removed after one hour
  2. additionWater (5 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 (5 mL)
  5. extractionthe desired product extracted with CHCl3 (2×20 mL)
  6. dry with materialThe combined organic extracts were dried (MgSO4)
  7. concentrationconcentrated under vacuum
  8. customPurification of the crude product by flash column chromatography

出典と根拠

ORDレコード
ord-489c760d37fb4af0a79cb7cedf0f9f40
出典データセット
uspto-grants-1997_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05661181

反応ノート

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