Benzaldehyde → HCID 10977131, 화합물

HRID 1267653노트

반응식

HRID 1267653 반응식
N[C@H](C=O)CCSC.[Na].[CH:10](=O)[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.[Br-].[Br:19][CH2:20][CH2:21][CH2:22][CH2:23][P+](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1>CC(O)C>[Br:19][CH2:20][CH2:21][CH2:22]/[CH:23]=[CH:10]/[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1

참가 물질

6

반응물 4

HCID 240BenzaldehydeHCID 446793Methionin ALHCID 2733851(4-Bromobutyl)triphenylphosphanium bromideHCID 5360545Sodium

생성물 1

HCID 10977131HCID 10977131, 화합물

시약·촉매·용매 1

HCID 3776Isopropanol용매

반응 조건

온도
70 °C

실험 절차

Metal sodium (303 mg) was added to dry 2-propanol (30 mL), and the mixture was stirred at 70° C. After the sodium was dissolved, benzaldehyde (1.0 g) was added to the solution at 0° C., 4-bromobutyltriphenylphosphonium bromide (5.4 g) was then added, and the mixture was gradually warmed to room temperature. After 5 hours, the reaction mixture was concentrated under reduced pressure, ethyl acetate was added to the residue, and the resultant mixture was washed with water and saturated brine, dried over anhydrous sodium sulfate and concentrated under reduced pressure. The residue was then purified by column chromatography on silica gel (hexane) to obtain the title compound.

후처리

  1. temperaturethe mixture was gradually warmed to room temperature
  2. concentrationthe reaction mixture was concentrated under reduced pressure, ethyl acetate
  3. additionwas added to the residue
  4. washthe resultant mixture was washed with water and saturated brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was then purified by column chromatography on silica gel (hexane)

출처 및 근거

ORD 기록
ord-9d2367d9d44b456fac0bc0d0bb752681
출처 데이터셋
uspto-grants-2003_04
특허 번호
US06552188B2

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