Thionyl Chloride → HCID 18448592、化合物

HRID 32050ノート

反応式

HRID 32050 の反応式
[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

参加物

4

反応物 2

HCID 24386Thionyl ChlorideHCID 184486127-Cyano-4-chromanol

生成物 1

HCID 18448592HCID 18448592、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
10 °C

実験手順

7-Cyano-4-chromanol (Step B) (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.

後処理

  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

出典と根拠

ORDレコード
ord-24b5b25dfecc4510886968d66f9bcdce
出典データセット
uspto-grants-2008_09
特許番号
US07425631B2

反応ノート

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