Pyridine → HCID 23126010、化合物

HRID 132737ノート

反応式

HRID 132737 の反応式
[CH2:1]([C:5]([CH2:10][CH:11]([CH3:13])[CH3:12])([CH2:8][OH:9])[CH2:6][OH:7])[CH:2]([CH3:4])[CH3:3].[O:14]1[CH2:18][CH2:17][CH2:16][CH2:15]1.N1C=C[CH:22]=[CH:21][CH:20]=1.[C:25](Cl)(=[O:32])[C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1>O>[C:18]([O:9][CH2:8][C:5]([CH2:10][CH:11]([CH3:13])[CH3:12])([CH2:1][CH:2]([CH3:4])[CH3:3])[CH2:6][O:7][C:25](=[O:32])[C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)(=[O:14])[C:17]1[CH:22]=[CH:21][CH:20]=[CH:15][CH:16]=1

参加物

6

反応物 4

HCID 1049PyridineHCID 7412Benzoyl chlorideHCID 8028TetrahydrofuranHCID 39856252,2-Diisobutyl-1,3-propanediol

生成物 1

HCID 23126010HCID 23126010、化合物収率 93%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To 7.5 g (0.04 mol) 2,2-diisobutyl-1,3-propandiol was added 50 ml tetrahydrofuran, then added 9.7 ml (0.12 mol) pyridine with stirring. To the resulting homogenous mixture was slowly added 11.6 ml (0.1 mol) benzoyl chloride. The mixture was stirred at room temperature for 1 hour, and heated refluxing for 5 hours. Upon completing the reaction, 40 ml water was added to dissolve the resulting salt. The mixture was extracted with ethyl acetate. The organic phase was separated, washed with saturated saline for two times, and dried over anhydrous sodium sulfate. The solvent was removed. Distillation under reduced pressure gave 2,2-diisobutyl-1,3-propandiol dibenzoate as a pale yellow liquid, the yield was 93%.

後処理

  1. stirringThe mixture was stirred at room temperature for 1 hour
  2. temperatureheated
  3. temperaturerefluxing for 5 hours
  4. additionwas added
  5. dissolutionto dissolve the resulting salt
  6. extractionThe mixture was extracted with ethyl acetate
  7. customThe organic phase was separated
  8. washwashed with saturated saline for two times
  9. dry with materialdried over anhydrous sodium sulfate
  10. customThe solvent was removed
  11. distillationDistillation under reduced pressure

出典と根拠

ORDレコード
ord-af2ac3dc5dd947b3a85b59d1d0d175ca
出典データセット
uspto-grants-2008_06
特許番号
US07388061B2

反応ノート

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