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Hydrochloric Acid → 6-(Tert-butoxycarbonyl)-3-propargyl-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidine-2,4-dione

HRID 1500605
ノート
印刷プレビュー

反応式

HRID 1500605 の反応式
C(O[C:4]([C:6]1[CH2:7][N:8]([C:22]([O:24][C:25]([CH3:28])([CH3:27])[CH3:26])=[O:23])[CH2:9][CH2:10][C:11]=1[NH:12][C:13]([O:15]C1C=CC=CC=1)=O)=[O:5])C.[CH2:29]([NH2:32])[C:30]#[CH:31].C1CCN2C(=NCCC2)CC1.NC(N)=O.[OH-].[Na+].Cl>C1COCC1>[C:25]([O:24][C:22]([N:8]1[CH2:9][CH2:10][C:11]2[NH:12][C:13](=[O:15])[N:32]([CH2:29][C:30]#[CH:31])[C:4](=[O:5])[C:6]=2[CH2:7]1)=[O:23])([CH3:26])([CH3:27])[CH3:28]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 6

HCID 313Hydrochloric AcidHCID 1176UreaHCID 14798Sodium HydroxideHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 239041PropargylamineHCID 66685805Ethyl-4-phenoxycarbonylamino-1-tert-butoxycarbonyl-1,2,5,6-tetrahydropyridine-3-carboxylate

生成物 1

HCID 86663112
6-(Tert-butoxycarbonyl)-3-propargyl-5,6,7,8-tetrahydropyrido[4,3-d]pyrimidine-2,4-dione

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Ethyl-4-phenoxycarbonylamino-1-tert-butoxycarbonyl-1,2,5,6-tetrahydropyridine-3-carboxylate (5.0 g) was dissolved in THF (50 ml), and propargylamine (1.32 ml) and 1,8-diazabicyclo[5.4.0]-7-undecene (DBU) (0.2 ml) were added and the resultant mixture was stirred at room temperature for 2 hours. After production of an intermediate (urea) was confirmed by TLC, a 5 N aqueous sodium hydroxide solution (5 ml) was added and the resultant mixture was further stirred at room temperature for 2 hours. To the reaction solution, 6 N hydrochloric acid was added to neutralize and the resultant mixture was then concentrated. To the residue, water was added and the mixture was extracted with ethyl acetate. After the organic layer was washed with a saturated saline solution, the organic layer was dried over sodium sulfate, filtrated and concentrated under reduced pressure. A precipitate was obtained by filtration. The titled compound (3.78 g) was obtained as a white powder.

後処理

  1. concentrationthe resultant mixture was then concentrated
  2. additionTo the residue, water was added
  3. extractionthe mixture was extracted with ethyl acetate
  4. washAfter the organic layer was washed with a saturated saline solution
  5. dry with materialthe organic layer was dried over sodium sulfate
  6. filtrationfiltrated
  7. concentrationconcentrated under reduced pressure
  8. customA precipitate was obtained by filtration

出典と根拠

ORDレコード
ord-aee827a40f924f74985411118979f327
出典データセット
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09206173B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート