Sodium Acetate → HCID 86654801、化合物

HRID 521530ノート

反応式

HRID 521530 の反応式
[CH:1]([C:3]1[CH:4]=[C:5]([CH:9]=[CH:10][C:11]=1[O:12][CH3:13])[C:6]([OH:8])=O)=[O:2].Cl.[CH3:15][O:16][C:17]([C:19]1([NH2:28])[CH2:27][C:26]2[C:21](=[CH:22][CH:23]=[CH:24][CH:25]=2)[CH2:20]1)=[O:18].C([O-])(=O)C.[Na+]>C(O)(=O)C>[CH3:15][O:16][C:17]([C:19]1([NH:28][C:6](=[O:8])[C:5]2[CH:9]=[CH:10][C:11]([O:12][CH3:13])=[C:3]([CH:1]=[O:2])[CH:4]=2)[CH2:27][C:26]2[C:21](=[CH:22][CH:23]=[CH:24][CH:25]=2)[CH2:20]1)=[O:18]

参加物

5

反応物 3

HCID 517045Sodium AcetateHCID 190399693-Formyl-4-methoxybenzoic acidHCID 45074056methyl 2-amino-2,3-dihydro-1H-indene-2-carboxylate hydrochloride

生成物 1

HCID 86654801HCID 86654801、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

3-Formyl-4-methoxy-benzoic acid (F. D. Chattaway and F. Calvet, J. Chem. Soc. (1928), 2913-2918) (1.017 g, 5.65 mmol) was reacted with 2-amino-indane-2-carboxylic acid methyl ester hydrochloride in analogy to step 4 of example 3. The obtained product (1.895 g) was dissolved in acetic acid (20 ml), sodium acetate (0.57 g, 6.96 mmol) was added and the mixture was stirred under reflux for 24 h. The volatiles were evaporated in vacuo, the residue partitioned between a saturated sodium hydrogencarbonate solution and EA, and the aqueous phase extracted with EA. The combined organic phases were dried over sodium sulfate and evaporated to dryness to yield 1.52 g of the title compound.

後処理

  1. temperatureunder reflux for 24 h
  2. customThe volatiles were evaporated in vacuo
  3. customthe residue partitioned between a saturated sodium hydrogencarbonate solution and EA
  4. extractionthe aqueous phase extracted with EA
  5. dry with materialThe combined organic phases were dried over sodium sulfate
  6. customevaporated to dryness

出典と根拠

ORDレコード
ord-815455bc569a4d7ca80ecaaa5701bee1
出典データセット
uspto-grants-2016_05
特許番号
US09328071B2

反応ノート

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