Acetic Acid → HCID 178457008、化合物

HRID 80003

反応式

HRID 80003 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-5d84672327704de68b2ec07c7ee9aeb1
出典データセット
uspto-grants-2014_09
特許番号
USRE045174E1

関連ノート

読み込み中…