Sodium Chloride → 4-(1-Pyrrolyl)-2-indanyl acetate

HRID 1164209ノート

反応式

HRID 1164209 の反応式
[C:1]([O:4][CH:5]1[CH2:13][C:12]2[C:7](=[CH:8][CH:9]=[CH:10][C:11]=2[NH2:14])[CH2:6]1)(=[O:3])[CH3:2].CO[CH:17]1[CH2:21][CH2:20][CH:19](OC)O1.C(Cl)(Cl)Cl.[Cl-].[Na+]>C(O)(=O)C>[C:1]([O:4][CH:5]1[CH2:13][C:12]2[C:7](=[CH:8][CH:9]=[CH:10][C:11]=2[N:14]2[CH:17]=[CH:21][CH:20]=[CH:19]2)[CH2:6]1)(=[O:3])[CH3:2]

参加物

6

反応物 4

HCID 5234Sodium ChlorideHCID 6212ChloroformHCID 790982,5-DimethoxytetrahydrofuranHCID 132395844-amino-2,3-dihydro-1H-inden-2-yl acetate

生成物 1

HCID 132395854-(1-Pyrrolyl)-2-indanyl acetate収率 92.2%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A stirred solution of 0.70 g (0.004 mole) of 4-amino-2-indanyl acetate and 0.56 g (0.004 mole) of 2,5-dimethoxytetrahydrofuran in 1.5 mL of acetic acid was heated under reflux for 3 hours. The reaction mixture was cooled to ambient temperature and poured into 30 mL of chloroform. The mixture was stirred with 30 mL of an aqueous saturated solution of sodium chloride. The organic layer was removed, and the aqueous layer extracted with two portions of 30 mL each of chloroform. The combined organic phases were washed with two portions of 30 mL each of an aqueous saturated solution of sodium chloride. The organic layer was dried over potassium carbonate, filtered, and the filtrate concentrated under reduced pressure to give 0.89 g of 4-(1-pyrrolyl)-2-indanyl acetate.

後処理

  1. temperatureunder reflux for 3 hours
  2. customThe organic layer was removed
  3. extractionthe aqueous layer extracted with two portions of 30 mL each of chloroform
  4. washThe combined organic phases were washed with two portions of 30 mL each of an aqueous saturated solution of sodium chloride
  5. dry with materialThe organic layer was dried over potassium carbonate
  6. filtrationfiltered
  7. concentrationthe filtrate concentrated under reduced pressure

出典と根拠

ORDレコード
ord-f48efcd4498e405eb6902c35614bd0c4
出典データセット
uspto-grants-1983_01
特許番号
US04368205

反応ノート

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