Acetic Acid → HCID 178457008、化合物

HRID 254847

反応式

HRID 254847 の反応式
[C:1]1([N:7]2[C:11](=[O:12])[CH2:10][S:9]/[C:8]/2=[N:13]\[CH:14]([CH3:16])[CH3:15])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:17]([O-:20])(=[O:19])C.[Na+].[C:22](O)(=O)[CH3:23]>CC(=O)OCC>[O:19]1[C:1]2[CH:6]=[CH:5][C:22](/[CH:23]=[C:10]3/[C:11](=[O:12])[N:7]([C:1]4[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=4)/[C:8](=[N:13]/[CH:14]([CH3:16])[CH3:15])/[S:9]/3)=[CH:3][C:2]=2[O:20][CH2:17]1

参加物

5

反応物 3

HCID 176Acetic AcidHCID 517045Sodium AcetateHCID 178457009HCID 178457009、化合物

生成物 1

HCID 178457008HCID 178457008、化合物

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

A solution of 3-phenyl-2-[(Z)-isopropylimino]-thiazolidin-4-one (150 mg, 0.64 mmol), piperonat (192 mg, 1.28 mmol) and sodium acetate (105 mg, 1.28 mmol) in acetic acid (3 mL) is stirred at 110° C. for 4 h. The dark yellow to brown solution is cooled to rt, diluted with EA (75 mL), washed with sat. aq. NaHCO3, followed by water, and evaporated. The crude product is purified by crystallisation from a small amount of methanol (approx. 5 mL) to give 5-benzo[1,3]dioxol-5-ylmeth-(Z)-ylidene-2-[(Z)-isopropylimino]-3-phenyl-thiazolidin-4-one.

後処理

  1. washwashed with sat. aq. NaHCO3
  2. customevaporated
  3. customThe crude product is purified by crystallisation from a small amount of methanol (approx. 5 mL)

出典と根拠

ORDレコード
ord-4ee8e094ddee4826829e646438f5b822
出典データセット
uspto-grants-2011_01
特許番号
US07875726B2

関連ノート

読み込み中…