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Hydrochloric Acid → HCID 21487254、化合物

HRID 1414380
ノート
印刷プレビュー

反応式

HRID 1414380 の反応式
[Cl:1][CH2:2][CH2:3][O:4][CH:5]1[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[C:7](=[O:14])[N:6]1[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1.O.[OH-].[Na+].Cl>C(N)(C)C.CC(C)=O.C(OCC)C>[ClH:1].[CH:15]([NH:6][CH2:2][CH2:3][O:4][CH:5]1[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[C:7](=[O:14])[N:6]1[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)([CH3:20])[CH3:16]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 14798Sodium Hydroxide2 回HCID 21487243HCID 21487243、化合物

生成物 1

HCID 21487254HCID 21487254、化合物

試薬・触媒・溶媒 3

HCID 180Acetone溶媒HCID 3283
Diethyl Ether
溶媒
HCID 6363Isopropylamine溶媒

実験手順

A solution of 3-(2-chloroethoxy)-2-phenyl-isoindolin-1-one in isopropylamine (120cc.) is heated in an autoclave at 120°C. for 24 hours. After cooling, the reaction mixture is poured into water (200 cc.) and 4N sodium hydroxide solution (16 cc.). The alkaline solution obtained is extracted with diethyl ether (250 cc.). The organic solution is washed with water (3 × 50 cc.) and is then extracted with 4N hydrochloric acid (18 cc.). The acid solution obtained is rendered alkaline by adding 4N sodium hydroxide solution (20 cc.) and the oily product which separates out is extracted with diethyl ether (2 × 100 cc.). The organic extracts are then dried over sodium sulphate and concentrated to dryness under reduced pressure. A product (14.2 g.), which melts at about 85°C., is obtained and is dissolved in acetone (150 cc.). A 4.03N solution of hydrogen chloride in diethyl ether (11.3 cc.) is added to the resulting solution. The product which crystallises is filtered off and then washed with acetone (10 cc.). After drying, 3-(2-isopropylaminoethoxy)-2-phenyl-isoindolin-1-one hydrochloride (11.3 g.), which melts at 184° C., is obtained.

後処理

  1. temperatureAfter cooling
  2. customThe alkaline solution obtained
  3. extractionis extracted with diethyl ether (250 cc.)
  4. washThe organic solution is washed with water (3 × 50 cc.)
  5. extractionis then extracted with 4N hydrochloric acid (18 cc.)
  6. customThe acid solution obtained
  7. extractionthe oily product which separates out is extracted with diethyl ether (2 × 100 cc.)
  8. dry with materialThe organic extracts are then dried over sodium sulphate
  9. concentrationconcentrated to dryness under reduced pressure
  10. customA product (14.2 g.), which melts at about 85°C., is obtained
  11. customThe product which crystallises
  12. filtrationis filtered off
  13. washwashed with acetone (10 cc.)
  14. customAfter drying

出典と根拠

ORDレコード
ord-937c92cba1d64c009bb45b24746fbfed
出典データセット
uspto-grants-1977_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04001271

反応ノート

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