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Water → 1H-Purine-2,6-dione, 3,7-dihydro-8-(2-(4-(4-aminobutoxy)phenyl)ethenyl)-1,3-diethyl-7-methyl-,(E)-

HRID 375373
ノート
印刷プレビュー

反応式

HRID 375373 の反応式
[N:1]([CH2:4][CH2:5][CH2:6][CH2:7][O:8][C:9]1[CH:32]=[CH:31][C:12](/[CH:13]=[CH:14]/[C:15]2[N:23]([CH3:24])[C:22]3[C:21](=[O:25])[N:20]([CH2:26][CH3:27])[C:19](=[O:28])[N:18]([CH2:29][CH3:30])[C:17]=3[N:16]=2)=[CH:11][CH:10]=1)=[N+]=[N-].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.O.[OH-].[Na+]>O1CCCC1>[NH2:1][CH2:4][CH2:5][CH2:6][CH2:7][O:8][C:9]1[CH:10]=[CH:11][C:12](/[CH:13]=[CH:14]/[C:15]2[N:23]([CH3:24])[C:22]3[C:21](=[O:25])[N:20]([CH2:26][CH3:27])[C:19](=[O:28])[N:18]([CH2:29][CH3:30])[C:17]=3[N:16]=2)=[CH:31][CH:32]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 11776TriphenylphosphineHCID 14798Sodium HydroxideHCID 64489521H-Purine-2,6-dione, 3,7-dihydro-8-(2-(4-(4-azidobutoxy)phenyl)ethenyl)-1,3-diethyl-7-methyl-,(E)-

生成物 1

HCID 64489531H-Purine-2,6-dione, 3,7-dihydro-8-(2-(4-(4-aminobutoxy)phenyl)ethenyl)-1,3-diethyl-7-methyl-,(E)-

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒

実験手順

Compound 178 (75 mg, 0.17 mmol) obtained in Reference Example 117 was dissolved in 7.5 ml of tetrahydrofuran. To the solution was added 90 mg (0.34 mmol) of triphenylphosphine, and the mixture was heated under reflux for 3 hours. Water (5 ml) was added thereto and the mixture was heated under reflux for further one hour. After cooling, a 2N aqueous solution of sodium hydroxide was added thereto, and the mixture was extracted with chloroform and dried over anhydrous sodium sulfate, followed by evaporation under reduced pressure. The residue was purified by silica gel column chromatography (eluent: chloroform/methanol/triethylamine) to give 74 mg (yield quant.) of Compound 179. The obtained crude crystals were further recrystallized from 2-propanol/water.

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 3 hours
  3. temperaturethe mixture was heated
  4. temperatureunder reflux for further one hour
  5. temperatureAfter cooling
  6. extractionthe mixture was extracted with chloroform
  7. dry with materialdried over anhydrous sodium sulfate
  8. customfollowed by evaporation under reduced pressure
  9. customThe residue was purified by silica gel column chromatography (eluent: chloroform/methanol/triethylamine)
  10. customto give

出典と根拠

ORDレコード
ord-d0cb9c02f3de4062803f3cfc0e11e359
出典データセット
uspto-grants-1996_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05484920

反応ノート

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