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4-Chlorobutyryl chloride → HCID 57245589, 화합물

HRID 1066467
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인쇄 미리보기

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HRID 1066467 반응식
[Cl:1][CH2:2][CH2:3][CH2:4][C:5](Cl)=[O:6].[Al+3].[Cl-].[Cl-].[Cl-].[C:12]1([CH2:18][C:19]([O:21][CH2:22][CH:23]([CH2:28][CH3:29])[CH2:24][CH2:25][CH2:26][CH3:27])=[O:20])[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1>>[Cl:1][CH2:2][CH2:3][CH2:4][C:5]([C:15]1[CH:16]=[CH:17][C:12]([CH2:18][C:19]([O:21][CH2:22][CH:23]([CH2:28][CH3:29])[CH2:24][CH2:25][CH2:26][CH3:27])=[O:20])=[CH:13][CH:14]=1)=[O:6]
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참가 물질

4

반응물 3

HCID 783704-Chlorobutyryl chlorideHCID 2217172-Ethylhexyl phenylacetateHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 57245589HCID 57245589, 화합물

반응 조건

온도
35 °C

실험 절차

Mix chlorobutyryl chloride (16.9 g) and AlCl3 (29.3 g) at room temperature. Add 2-phenylacetic acid, 2-ethylhexyl ester (27.6 g), keeping the temperature below 10° C. Heat at 35° C. for 24 hours, quench in ice water (200 g). Separate the organic phase, dry (MgSO4) and evaporate the solvent in vacuo. Dilute the residue with ethanol (150 mL), add hydrogen chloride (5 g) and heat to 75° C. After 2.5 hours, add another 5 g of hydrogen chloride and stir at 75° C. for 24 hours. Evaporate the solvent in vacuo to give the title compound.

후처리

  1. customthe temperature below 10° C
  2. customquench in ice water (200 g)
  3. customSeparate the organic phase
  4. dry with materialdry (MgSO4)
  5. customevaporate the solvent in vacuo
  6. additionDilute the residue with ethanol (150 mL)
  7. additionadd hydrogen chloride (5 g)
  8. temperatureheat to 75° C
  9. additionadd another 5 g of hydrogen chloride
  10. customEvaporate the solvent in vacuo

출처 및 근거

ORD 기록
ord-98470ae173be4c65a568e5f317d57c5a
출처 데이터셋
uspto-grants-2001_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06242606B1

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