Hydrochloric Acid → Methyl 4-(2-acetylaminophenyl)butanoate

HRID 1242902

反応式

HRID 1242902 の反応式
Cl.[NH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[CH2:9][CH2:10][CH2:11][C:12]([O:14][CH3:15])=[O:13].C(N(CC)CC)C.[C:23](Cl)(=[O:25])[CH3:24].Cl>O1CCCC1.C(OCC)(=O)C>[C:23]([NH:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[CH2:9][CH2:10][CH2:11][C:12]([O:14][CH3:15])=[O:13])(=[O:25])[CH3:24]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 6367Acetyl chlorideHCID 8471TriethylamineHCID 21940035Methyl 4-(2-aminophenyl)butanoate hydrochloride

生成物 1

HCID 21939908Methyl 4-(2-acetylaminophenyl)butanoate収率 73.5%

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

実験手順

Methyl 4-(2-aminophenyl)butanoate hydrochloride (7.20 g, 0.037 mol) synthesized by a known method by documents (Synthetic communications, 26(18), 3443 (1996)) and triethylamine (5.06 g, 0.05 mol) were dissolved in tetrahydrofuran (60 ml). Acetyl chloride (3.51 g, 0.045 mol) was added dropwise to the mixture, which was stirred at room temperature for 30 minutes. Ethyl acetate and 1N hydrochloric acid were added to the reaction mixture, and extraction was conducted. The organic layer was washed with water, concentrated and dried. A mixed solution of ethyl acetate-n-hexane (1:1) was added to the residue. The crystallized product was collected by filtration, to give methyl 4-(2-acetylaminophenyl)butanoate (6.40 g) as a white powder.

後処理

  1. washThe organic layer was washed with water
  2. concentrationconcentrated
  3. customdried
  4. additionA mixed solution of ethyl acetate-n-hexane (1:1) was added to the residue
  5. filtrationThe crystallized product was collected by filtration

出典と根拠

ORDレコード
ord-8965cf46fabd464d87d6ed70456b2500
出典データセット
uspto-grants-2006_10
特許番号
US07115750B1

関連ノート

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