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Hydrochloric Acid → HCID 57860414、化合物

HRID 1947114
ノート
印刷プレビュー

反応式

HRID 1947114 の反応式
[O-]CC.[Na+].[C:5]([O:9][CH2:10][CH3:11])(=[O:8])[CH2:6][SH:7].[Cl:12][C:13]1[C:18]([C:19](OCC)=[O:20])=[C:17](Cl)[C:16]([CH3:25])=[C:15]([CH3:26])[N:14]=1.Cl>C(O)C>[Cl:12][C:13]1[C:18]2[C:19]([OH:20])=[C:6]([C:5]([O:9][CH2:10][CH3:11])=[O:8])[S:7][C:17]=2[C:16]([CH3:25])=[C:15]([CH3:26])[N:14]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 12185Ethyl ThioglycolateHCID 2723922Sodium ethoxideHCID 12749674Ethyl 2,4-dichloro-5,6-dimethylnicotinate

生成物 1

HCID 57860414HCID 57860414、化合物収率 52%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

A 20% solution (1.73 g, 5.08 mmol) of sodium ethoxide in ethanol was diluted with ethanol (5 mL), and ethyl thioglycolate (610 mg, 5.08 mmol) was added. Ethyl 2,4-dichloro-5,6-dimethylpyridine-3-carboxylate (630 mg, 2.54 mmol) was added to the mixture, and the mixture was stirred at room temperature for 18 hr. 2N Hydrochloric acid (3 mL) was added to the reaction mixture and the mixture was partitioned between brine and ethyl acetate. The organic layer was dried over magnesium sulfate and concentrated. The obtained solid was washed with diisopropyl ether-hexane, and dried under reduced pressure to give the title compound (374 mg, 52%) as a white powder.

後処理

  1. additionwas added
  2. customthe mixture was partitioned between brine and ethyl acetate
  3. dry with materialThe organic layer was dried over magnesium sulfate
  4. concentrationconcentrated
  5. washThe obtained solid was washed with diisopropyl ether-hexane
  6. customdried under reduced pressure

出典と根拠

ORDレコード
ord-127fb91e6f1f4fcd8b7014b5428a8901
出典データセット
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08399449B2

反応ノート

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