Isopropanol → Acetic acid, (p-aminobenzoyl)-, ethyl ester (6CI,7CI)

HRID 542401

反応式

HRID 542401 の反応式
[Cl-].[NH4+].C(O)(C)C.[N+:7]([C:10]1[CH:23]=[CH:22][C:13]([C:14]([CH2:16][C:17]([O:19][CH2:20][CH3:21])=[O:18])=[O:15])=[CH:12][CH:11]=1)([O-])=O>O>[NH2:7][C:10]1[CH:11]=[CH:12][C:13]([C:14]([CH2:16][C:17]([O:19][CH2:20][CH3:21])=[O:18])=[O:15])=[CH:22][CH:23]=1

参加物

5

反応物 3

HCID 3776IsopropanolHCID 13281Benzenepropanoic acid, 4-nitro-beta-oxo-, ethyl esterHCID 25517Ammonium Chloride

生成物 1

HCID 3045879Acetic acid, (p-aminobenzoyl)-, ethyl ester (6CI,7CI)収率 83.1%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
5 °C

実験手順

A mixture of 224 g of reduced iron, 13.4 g of ammonium chloride, 1,000 ml of isopropyl alcohol, and 200 ml of water was prepared, and then 237 g of ethyl p-nitrobenzoylacetate was added thereto in small amounts at temperatures ranging between 50° and 70° C. They were reacted at 70° C. for 1 hour and then the reaction solution was filtered. Then, 1,000 ml of water was added to the filtrate and cooled to 5° C., and crystals precipitated were collected by filtration to yield 172 g of yellow ethyl p-aminobenzoylacetate crystals, m.p., 82°-4° C.

後処理

  1. customwas prepared
  2. customranging between 50° and 70° C
  3. customThey were reacted at 70° C. for 1 hour
  4. filtrationthe reaction solution was filtered
  5. additionThen, 1,000 ml of water was added to the filtrate
  6. customcrystals precipitated
  7. filtrationwere collected by filtration

出典と根拠

ORDレコード
ord-e2635a4e17704d4890f22ca506076b41
出典データセット
uspto-grants-1987_04
特許番号
US04657848

関連ノート

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