Hydrochloric Acid → HCID 21851265、化合物

HRID 617166ノート

反応式

HRID 617166 の反応式
[CH2:1]([O:3][C:4]1[CH:5]=[C:6]2[C:11](=[CH:12][C:13]=1[O:14][CH2:15][C:16]([O:18]CC)=[O:17])[N:10]=[C:9]([N:21]1[CH2:26][CH2:25][O:24][CH2:23][CH2:22]1)[N:8]=[C:7]2[N:27]1[CH2:32][CH2:31][CH:30]([N:33]2[C:42](=[O:43])[C:41]3[C:36](=[CH:37][CH:38]=[C:39]([CH3:44])[CH:40]=3)[N:35]([CH3:45])[C:34]2=[O:46])[CH2:29][CH2:28]1)[CH3:2].[OH-].[Na+].Cl.CCOCC>CO>[C:16]([CH2:15][O:14][C:13]1[CH:12]=[C:11]2[C:6]([C:7]([N:27]3[CH2:32][CH2:31][CH:30]([N:33]4[C:42](=[O:43])[C:41]5[C:36](=[CH:37][CH:38]=[C:39]([CH3:44])[CH:40]=5)[N:35]([CH3:45])[C:34]4=[O:46])[CH2:29][CH2:28]3)=[N:8][C:9]([N:21]3[CH2:26][CH2:25][O:24][CH2:23][CH2:22]3)=[N:10]2)=[CH:5][C:4]=1[O:3][CH2:1][CH3:2])([OH:18])=[O:17]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 3283Diethyl EtherHCID 14798Sodium HydroxideHCID 21851274HCID 21851274、化合物

生成物 1

HCID 21851265HCID 21851265、化合物収率 101.3%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

In 30 ml of methanol was dissolved 900 mg (1.42 mmol) of Compound 54 obtained in Example 54, 15 ml of 2N-sodium hydroxide was added, and the mixture was stirred under heating at reflux for 4 hour. After cooling, 4N-hydrochloric acid was added to the reaction mixture and the mixtute was neutralized and subjected to extraction with chloroform. The organic layer was washed, dried and concentrated to give the residue. Ether was added to the above residue to give the precipitate which was collected by filtration and dried to give 870 mg (yield: 100%) of Compound 56 as white crystals.

後処理

  1. additionwas added
  2. temperatureunder heating
  3. temperatureat reflux for 4 hour
  4. temperatureAfter cooling
  5. extractionsubjected to extraction with chloroform
  6. washThe organic layer was washed
  7. customdried
  8. concentrationconcentrated
  9. customto give the residue
  10. customto give the precipitate which
  11. filtrationwas collected by filtration
  12. customdried

出典と根拠

ORDレコード
ord-787565e4fbe248da9395e74212334636
出典データセット
uspto-grants-1999_09
特許番号
US05948784

反応ノート

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