Thionyl Chloride → HCID 18448592, 화합물

HRID 1269442노트

반응식

HRID 1269442 반응식
[C:1]([C:3]1[CH:12]=[C:11]2[C:6]([CH:7](O)[CH2:8][CH2:9][O:10]2)=[CH:5][CH:4]=1)#[N:2].O=S(Cl)[Cl:16]>C(Cl)Cl>[Cl:16][CH:7]1[C:6]2[C:11](=[CH:12][C:3]([C:1]#[N:2])=[CH:4][CH:5]=2)[O:10][CH2:9][CH2:8]1

참가 물질

4

반응물 2

HCID 24386Thionyl ChlorideHCID 184486127-Cyano-4-chromanol

생성물 1

HCID 18448592HCID 18448592, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
10 °C

실험 절차

7-Cyano-4-chromanol (8.0 g, 46 mmol) was dissolved in CH2Cl2 (120 mL) and cooled to 10° C. SOCl2 (5.0 mL, 70 mmol) was added, the reaction was warmed to RT and stirred overnight. The reaction was concentrated in vacuo and azeotroped with CH2Cl2 (2×50 mL). The residue was dissolved in EtOAc (500 mL), washed with saturated NaHCO3 (250 mL), and with brine (150 mL), dried over MgSO4, filtered and concentrated in vacuo to provide the title compound which was used without further purification.

후처리

  1. temperaturethe reaction was warmed to RT
  2. concentrationThe reaction was concentrated in vacuo
  3. customazeotroped with CH2Cl2 (2×50 mL)
  4. dissolutionThe residue was dissolved in EtOAc (500 mL)
  5. washwashed with saturated NaHCO3 (250 mL)
  6. dry with materialwith brine (150 mL), dried over MgSO4
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-ac3def4833c34bd5a0cc08b7b19e732f
출처 데이터셋
uspto-grants-2007_04
특허 번호
US07199244B2

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