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 55051ノート

反応式

HRID 55051 の反応式
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]

参加物

5

反応物 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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-859b81e30cc24fbb8f40579742bb0c79
出典データセット
uspto-grants-1997_04
特許番号
US05624926

反応ノート

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