Pyridine → HCID 86725330、化合物

HRID 925217ノート

反応式

HRID 925217 の反応式
[CH2:1]([O:3][C:4]([N:6]1[CH2:23][CH2:22][C:10]2[C:11]3[C:12](O)([CH3:20])[C:13]([F:19])([F:18])[CH2:14][C:15]=3[CH:16]=[CH:17][C:9]=2[CH2:8][CH2:7]1)=[O:5])[CH3:2].N1C=CC=CC=1.O=S(Cl)[Cl:32]>>[CH2:1]([O:3][C:4]([N:6]1[CH2:23][CH2:22][C:10]2[C:11]3[C:12]([Cl:32])([CH3:20])[C:13]([F:19])([F:18])[CH2:14][C:15]=3[CH:16]=[CH:17][C:9]=2[CH2:8][CH2:7]1)=[O:5])[CH3:2]

参加物

4

反応物 3

HCID 1049PyridineHCID 24386Thionyl ChlorideHCID 86725331HCID 86725331、化合物

生成物 1

HCID 86725330HCID 86725330、化合物

反応条件

温度
50 °C

実験手順

Into a glass vial containing the product from step (a) (231 mg, 0.710 mmol) dissolved in SOCl2 (2 ml), pyridine (1 μL, 0.0071 mmol) was added. The stirred reaction mixture was heated to 50° C. for 30 minutes. The volatiles were evaporated in vacuo and the residue diluted with water (50 ml). The aqueous mixture was extracted with EtOAc (3×). The combined EtOAc extracts were washed with brine, dried over Na2SO4, and solvent evaporated in vacuo to give the sub-title compound as a dark yellow oil (214 mg) that was used without further purification. MS: ESI (positive): 344 (M+1).

後処理

  1. customThe stirred reaction mixture
  2. customThe volatiles were evaporated in vacuo
  3. additionthe residue diluted with water (50 ml)
  4. extractionThe aqueous mixture was extracted with EtOAc (3×)
  5. washThe combined EtOAc extracts were washed with brine
  6. dry with materialdried over Na2SO4, and solvent
  7. customevaporated in vacuo

出典と根拠

ORDレコード
ord-4e946bf124194e16a27d81288b4929c6
出典データセット
uspto-grants-2016_03
特許番号
US09284277B2

反応ノート

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