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Guanidine Hydrochloride → 2,4,6-Triamino-5-[3-(naphth-1-yl)propyl]pyrimidine

HRID 440967
ノート
印刷プレビュー

反応式

HRID 440967 の反応式
[O-]CC.[Na+].[Na].Cl.[NH2:7][C:8]([NH2:10])=[NH:9].[C:11]([CH:13]([CH2:16][CH2:17][CH2:18][C:19]1[C:28]2[C:23](=[CH:24][CH:25]=[CH:26][CH:27]=2)[CH:22]=[CH:21][CH:20]=1)[C:14]#[N:15])#[N:12]>C(O)C>[NH2:9][C:8]1[N:10]=[C:14]([NH2:15])[C:13]([CH2:16][CH2:17][CH2:18][C:19]2[C:28]3[C:23](=[CH:24][CH:25]=[CH:26][CH:27]=3)[CH:22]=[CH:21][CH:20]=2)=[C:11]([NH2:12])[N:7]=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 5742Guanidine HydrochlorideHCID 2723922Sodium ethoxideHCID 5360545SodiumHCID 199555442-Cyano-5-(naphth-1-yl)pentanenitrile

生成物 1

HCID 199555012,4,6-Triamino-5-[3-(naphth-1-yl)propyl]pyrimidine

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of sodium ethoxide, prepared from 0.04 gram (0.002 mole) of sodium metal in 50 mL of ethanol, was stirred, and 0.2 gram (0.002 mole) of guanidine hydrochloride was added in one portion. The reaction mixture was stirred for 15 minutes and filtered to remove a precipitate. The filtrate was stirred, and 0.4 gram (0.002 mole) of 2-cyano-5-(naphth-1-yl)pentanenitrile was added in one portion. Upon completion of addition, the reaction mixture was heated at reflux for about 16 hours. After this time the reaction mixture was concentrated under reduced pressure to a residue. The residue was triturated with warm water, yielding, when dried, 0.4 gram of 2,4,6-triamino-5-[3-(naphth-1-yl)propyl]-pyrimidine, mp 181°-183° C., (dec.). The NMR spectrum was consistent with the proposed structure.

後処理

  1. stirringThe reaction mixture was stirred for 15 minutes
  2. filtrationfiltered
  3. customto remove a precipitate
  4. stirringThe filtrate was stirred
  5. additionUpon completion of addition
  6. temperaturethe reaction mixture was heated
  7. temperatureat reflux for about 16 hours
  8. concentrationAfter this time the reaction mixture was concentrated under reduced pressure to a residue
  9. customThe residue was triturated with warm water
  10. customyielding
  11. customwhen dried

出典と根拠

ORDレコード
ord-884a174be3224f5c9e9481173a64c3ec
出典データセット
uspto-grants-1996_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05521192

反応ノート

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