Hydrochloric Acid → 3-[1-(7-Carboxymethyloxy-6-methoxy-4-quinazolinyl)-4-piperidinyl]-1,2,3,4-tetrahydro-1,6-dimethyl-2,4-dioxo-quinazoline

HRID 2257747노트

반응식

HRID 2257747 반응식
C([O:3][C:4]([CH2:6][O:7][C:8]1[CH:17]=[C:16]2[C:11]([C:12]([N:18]3[CH2:23][CH2:22][CH:21]([N:24]4[C:33](=[O:34])[C:32]5[C:27](=[CH:28][CH:29]=[C:30]([CH3:35])[CH:31]=5)[N:26]([CH3:36])[C:25]4=[O:37])[CH2:20][CH2:19]3)=[N:13][CH:14]=[N:15]2)=[CH:10][C:9]=1[O:38][CH3:39])=[O:5])C.[OH-].[Na+].Cl>CO>[C:4]([CH2:6][O:7][C:8]1[CH:17]=[C:16]2[C:11]([C:12]([N:18]3[CH2:19][CH2:20][CH:21]([N:24]4[C:33](=[O:34])[C:32]5[C:27](=[CH:28][CH:29]=[C:30]([CH3:35])[CH:31]=5)[N:26]([CH3:36])[C:25]4=[O:37])[CH2:22][CH2:23]3)=[N:13][CH:14]=[N:15]2)=[CH:10][C:9]=1[O:38][CH3:39])([OH:5])=[O:3]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 229234383-[1-(7-Ethoxycarbonylmethoxy-6-methoxy-4-quinazolinyl)-4-piperidinyl]-1,2,3,4-tetrahydro-1,6-dimethyl-2,4-dioxoquinazoline

생성물 1

HCID 229234763-[1-(7-Carboxymethyloxy-6-methoxy-4-quinazolinyl)-4-piperidinyl]-1,2,3,4-tetrahydro-1,6-dimethyl-2,4-dioxo-quinazoline수율 33%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

In 10 ml of methanol was dissolved 250.0 mg (0.47 mmol) of Compound 93 obtained in Example 84, and 5 ml of a 2N aqueous solution of sodium hydroxide was added thereto, followed by heating under reflux for 6 hours. After cooling, the reaction mixture was neutralized by addition of 4N hydrochloric acid, and extracted with chloroform. The organic layer was washed and dried, and the solvent was distilled off under reduced pressure. To the residue was added ether, and the precipitated crystals were collected by filtration and dried to give 77.8 mg (yield: 33%) of Compound 95 as white crystals.

후처리

  1. additionwas added
  2. temperatureby heating
  3. temperatureunder reflux for 6 hours
  4. temperatureAfter cooling
  5. extractionextracted with chloroform
  6. washThe organic layer was washed
  7. customdried
  8. distillationthe solvent was distilled off under reduced pressure
  9. additionTo the residue was added ether
  10. filtrationthe precipitated crystals were collected by filtration
  11. customdried

출처 및 근거

ORD 기록
ord-b121a048092f437aa5164ea0cb3c6521
출처 데이터셋
uspto-grants-1997_08
특허 번호
US05658917

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