Water → HCID 86682561, 화합물

HRID 1469140노트

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HRID 1469140 반응식
[OH:1][CH2:2][CH2:3][CH2:4][CH2:5][C:6]([O:8][CH2:9][CH3:10])=[O:7].[Cl:11][C:12](Cl)([O:14]C(=O)OC(Cl)(Cl)Cl)Cl.N1C=CC=CC=1.O>C(Cl)Cl>[Cl:11][C:12]([O:1][CH2:2][CH2:3][CH2:4][CH2:5][C:6]([O:8][CH2:9][CH3:10])=[O:7])=[O:14]

참가 물질

6

반응물 4

HCID 962WaterHCID 1049PyridineHCID 94429TriphosgeneHCID 12917181Ethyl 5-hydroxypentanoate

생성물 1

HCID 86682561HCID 86682561, 화합물수율 179.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

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온도
0 °C

실험 절차

Ethyl 5-hydroxypentanoate (1.12 g, 7.66 mmol) was dissolved in 25 mL of methylene chloride, triphosgene (772 mg, 0.34 equivalent), and pyridine (0.743 mL, 1.2 equivalent) were sequentially added while stirred at 0° C., and the mixture was stirred at room temperature for 1 hour. After completion of the reaction, water was added, and extraction operation (methylene chloride) was performed. The separated organic layer was washed using an aqueous saturated sodium chloride solution, and dried with magnesium sulfate, and the solvent was distilled off under reduced pressure to obtain the crude product. This was purified by column chromatography (ethyl acetate:n-hexane=1:10) to obtain the title compound (972 mg) having the following physical property values.

후처리

  1. stirringthe mixture was stirred at room temperature for 1 hour
  2. additionwas added
  3. extractionextraction operation (methylene chloride)
  4. washThe separated organic layer was washed
  5. dry with materialdried with magnesium sulfate
  6. distillationthe solvent was distilled off under reduced pressure
  7. customto obtain the crude product
  8. customThis was purified by column chromatography (ethyl acetate:n-hexane=1:10)

출처 및 근거

ORD 기록
ord-a38eb0cbc66f43bf8ca5aabdc4c4077d
출처 데이터셋
uspto-grants-2015_04
특허 번호
US09006246B2

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