Piperonal → HCID 178457008、化合物

HRID 2061273

反応式

HRID 2061273 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.[CH:17]1[C:22]([CH:23]=O)=[CH:21][C:20]2[O:25][CH2:26][O:27][C:19]=2[CH:18]=1.C([O-])(=O)C.[Na+]>C(O)(=O)C.CC(=O)OCC>[O:27]1[C:19]2[CH:18]=[CH:17][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:21][C:20]=2[O:25][CH2:26]1

参加物

6

反応物 3

HCID 8438PiperonalHCID 517045Sodium AcetateHCID 178457009HCID 178457009、化合物

生成物 1

HCID 178457008HCID 178457008、化合物

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒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), piperonal (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-3aca3b1da28a4aebaf3a66508b47c36f
出典データセット
uspto-grants-2012_10
特許番号
USRE043728E1

関連ノート

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