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Neopentyl glycol → HCID 20323933、化合物

HRID 839717
ノート
印刷プレビュー

反応式

HRID 839717 の反応式
[CH3:1][C:2]([CH3:7])([CH2:5][OH:6])[CH2:3][OH:4].[C:8]([C:11]1[CH:19]=[CH:18][C:14]([C:15](Cl)=[O:16])=[CH:13][CH:12]=1)([OH:10])=[O:9]>N1C=CC=CC=1>[CH3:1][C:2]([CH3:7])([CH2:5][O:6][C:15]([C:14]1[CH:18]=[CH:19][C:11]([C:8]([OH:10])=[O:9])=[CH:12][CH:13]=1)=[O:16])[CH2:3][O:4][C:15]([C:14]1[CH:18]=[CH:19][C:11]([C:8]([OH:10])=[O:9])=[CH:12][CH:13]=1)=[O:16]
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 31344Neopentyl glycolHCID 123403414-(Chlorocarbonyl)benzoic acid

生成物 1

HCID 20323933HCID 20323933、化合物収率 80.4%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A mechanically stirred mixture of 15.6 g (0.15 M) of 2,2-dimethyl-1,3-propanediol, 92.25 g (0.5 M) of 4-carboxybenzoyl chloride and 500 ml of pyridine was refluxed under a nitrogen atmosphere. The resulting mixture was concentrated to dryness under reduced pressure, dispersed in 500 ml of distilled water, and acidified to pH 1 with concentrated hydrochloric acid. The precipitate was filtered off, washed three times with distilled water, and dried overnight at 100° C in a vacuum oven. The product was extracted for 5 days with 2 liters of hot benzene. The extract, on cooling, yielded 48.2 g of 4,4'-[(2,2-dimethyl-1,3-propanediyl)bis(oxycarbonyl)]bis(benzoic acid) melting at 287°-288° C. The infrared spectrum was consistent with the proposed structure and the compound was found to contain 5.13 meq of CO2H/g which corresponded to a molecular weight of 390 for the diacid.

後処理

  1. temperaturewas refluxed under a nitrogen atmosphere
  2. concentrationThe resulting mixture was concentrated to dryness under reduced pressure
  3. additiondispersed in 500 ml of distilled water
  4. filtrationThe precipitate was filtered off
  5. washwashed three times with distilled water
  6. customdried overnight at 100° C in a vacuum oven
  7. extractionThe product was extracted for 5 days with 2 liters of hot benzene
  8. temperatureThe extract, on cooling

出典と根拠

ORDレコード
ord-f137d5aa386e4d84a5ef962844b30cf2
出典データセット
uspto-grants-1978_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04096341

反応ノート

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