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Potassium Carbonate → HCID 58381715、化合物

HRID 410045
ノート
印刷プレビュー

反応式

HRID 410045 の反応式
C(=O)([S:3][CH2:4][CH2:5][CH2:6][CH2:7]/[CH:8]=[CH:9]\[CH2:10]/[CH:11]=[CH:12]\[CH2:13]/[CH:14]=[CH:15]\[CH2:16]/[CH:17]=[CH:18]\[CH2:19]/[CH:20]=[CH:21]\[CH2:22][CH3:23])C.C(=O)([O-])[O-].[K+].[K+]>CO>[CH2:4]([SH:3])[CH2:5][CH2:6][CH2:7]/[CH:8]=[CH:9]\[CH2:10]/[CH:11]=[CH:12]\[CH2:13]/[CH:14]=[CH:15]\[CH2:16]/[CH:17]=[CH:18]\[CH2:19]/[CH:20]=[CH:21]\[CH2:22][CH3:23]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 11430Potassium Carbonate2 回HCID 58381698HCID 58381698、化合物

生成物 1

HCID 58381715HCID 58381715、化合物収率 97.4%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

S-(5Z,8Z,11Z,14Z,17Z)-Icosa-5,8,11,14,17-pentaenyl ethanethioate (7.00 g, 20.2 mmol) was dissolved in MeOH (100 mL) by stirring 10 minutes until the droplets of oil dissolved, before anhydrous potassium carbonate, K2CO3 (2.79 g, 20.2 mmol) was added in one portion. The mixture was stirred for 1 hour and 20 minutes at ambient temperature and quenched by addition of 1 M HCl (50 mL) and water (150 mL). The white cloudy mixture was added Et2O (250 mL) and the phases were separated. The water phase was extracted with Et2O (2×250 mL). The combined organic phases were washed with brine (250 mL) and dried (MgSO4). Filtration and evaporation gave the title compound as oil (5.99 g, 97% yield), which was used without further purification.

後処理

  1. additionwas added in one portion
  2. stirringThe mixture was stirred for 1 hour and 20 minutes at ambient temperature
  3. customquenched by addition of 1 M HCl (50 mL) and water (150 mL)
  4. additionThe white cloudy mixture was added Et2O (250 mL)
  5. customthe phases were separated
  6. extractionThe water phase was extracted with Et2O (2×250 mL)
  7. washThe combined organic phases were washed with brine (250 mL)
  8. dry with materialdried (MgSO4)
  9. filtrationFiltration and evaporation

出典と根拠

ORDレコード
ord-16c188dbacfa4354b82fe5e19097bce1
出典データセット
uspto-grants-2014_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08759558B2

反応ノート

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