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

HRID 241798

反応式

HRID 241798 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
0 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-5cf7702b30e542609a21199f2ff478a7
出典データセット
uspto-grants-2014_02
特許番号
US08653081B2

関連ノート

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