Hydrochloric Acid → HCID 19439680, 화합물

HRID 1734021노트

반응식

HRID 1734021 반응식
O.NN.C1(=O)[N:8]([CH2:9][C:10]2[CH:11]=[C:12]([C:18](=[O:20])[CH3:19])[CH:13]=[CH:14][C:15]=2[O:16][CH3:17])C(=O)C2=CC=CC=C12.Cl>CO.O1CCCC1>[NH2:8][CH2:9][C:10]1[CH:11]=[C:12]([C:18](=[O:20])[CH3:19])[CH:13]=[CH:14][C:15]=1[O:16][CH3:17]

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 24654Hydrazine hydrate (1:1)HCID 3922617HCID 3922617, 화합물

생성물 1

HCID 19439680HCID 19439680, 화합물수율 48.8%

시약·촉매·용매 2

HCID 887Methanol용매HCID 8028Tetrahydrofuran용매

실험 절차

Hydrazine hydrate (3.06 g) was added to a suspension of 3'-phthalimidomethyl-4'-methoxyacetophenone (15.74 g) in methanol (150 ml) and tetrahydrofuran (150 ml) at room temperature and the mixture was stirred at room temperature for 24 hours. Dilute hydrochloric acid (conc. hydrochloric acid (5 ml) in water (100 ml)) was added slowly to the mixture with cooling and the mixture was stirred at room temperature for 1 hour. The mixture was concentrated. Water (100 ml) was added thereto and the mixture was alkalized to pH 10 with 30% aqueous potassium carbonate solution and extracted with ethyl acetate (300 ml). The extract was dried with magnesium sulfate. The solvent was removed under reduced pressure to afford 3'-aminomethyl-4'-methoxyacetophenone (4.45 g).

후처리

  1. temperaturewith cooling
  2. stirringthe mixture was stirred at room temperature for 1 hour
  3. concentrationThe mixture was concentrated
  4. additionWater (100 ml) was added
  5. extractionextracted with ethyl acetate (300 ml)
  6. dry with materialThe extract was dried with magnesium sulfate
  7. customThe solvent was removed under reduced pressure

출처 및 근거

ORD 기록
ord-09db1c266b91498285a83bd0b0c0e292
출처 데이터셋
uspto-grants-1996_07
특허 번호
US05532258

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