Thionyl Chloride → 1-chloro-4-nitro-2,3-dihydro-1H-indene

HRID 241798

반응식

HRID 241798 반응식
[N+:1]([C:4]1[CH:12]=[CH:11][CH:10]=[C:9]2[C:5]=1[CH2:6][CH2:7][CH:8]2O)([O-:3])=[O:2].S(Cl)([Cl:16])=O>C1(C)C=CC=CC=1>[Cl:16][CH:8]1[C:9]2[C:5](=[C:4]([N+:1]([O-:3])=[O:2])[CH:12]=[CH:11][CH:10]=2)[CH2:6][CH2:7]1

참가 물질

4

반응물 2

HCID 24386Thionyl ChlorideHCID 131024564-Nitro-2,3-dihydro-1H-inden-1-OL

생성물 1

HCID 593027291-chloro-4-nitro-2,3-dihydro-1H-indene

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
0 °C

실험 절차

To a 0° C. solution of 4-nitro-2,3-dihydro-1H-inden-1-ol (252 mg, 1.41 mmol, 1.0 equiv) in dry toluene (2.5 mL) was added thionyl chloride (160 μL, 2.11 mmol, 1.5 equiv) dropwise by syringe. After stirring at 0° C. for 30 min, the reaction mixture was heated to 55° C. for 2 h. The reaction was allowed to cool to room temperature, washed twice with water, dried over sodium sulfate, filtered and concentrated in vacuo. The unpurified alkyl chloride (221 mg, 79%) was used without further purification.

후처리

  1. temperaturethe reaction mixture was heated to 55° C. for 2 h
  2. temperatureto cool to room temperature
  3. washwashed twice with water
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customThe unpurified alkyl chloride (221 mg, 79%) was used without further purification

출처 및 근거

ORD 기록
ord-5cf7702b30e542609a21199f2ff478a7
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08653081B2

연결된 노트

불러오는 중…