Sodium Acetate → HCID 86654801, 화합물

HRID 1810930노트

반응식

HRID 1810930 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 86654801HCID 86654801, 화합물

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-202f12e5254e458186b7c6b347eec8c8
출처 데이터셋
uspto-grants-2013_01
특허 번호
US08362073B2

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