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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Hydrochloric Acid → HCID 21487254, 화합물

HRID 1974365
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HRID 1974365 반응식
[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]
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참가 물질

8

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 14798Sodium Hydroxide2회HCID 21487243HCID 21487243, 화합물

생성물 1

HCID 21487254HCID 21487254, 화합물

시약·촉매·용매 3

HCID 180Acetone용매
HCID 3283
Diethyl Ether
용매
HCID 6363Isopropylamine용매

실험 절차

A solution of 3-(2-chloroethoxy)-2-phenyl-isoindolin-1-one in isopropylamine (120 cc.) 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 4.03 N 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.

후처리

  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

출처 및 근거

ORD 기록
ord-189c8bc972574c6a84932c8adc563dc9
출처 데이터셋
uspto-grants-1976_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04000306

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