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

HRID 1081639
ノート
印刷プレビュー

反応式

HRID 1081639 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. filtrationfiltered
  2. customto remove a precipitate
  3. stirringThe filtrate was stirred
  4. additionUpon completion of addition
  5. temperaturethe reaction mixture was heated
  6. temperatureat reflux for about 16 hours
  7. concentrationAfter this time the reaction mixture was concentrated under reduced pressure to a residue
  8. customThe residue was triturated with warm water
  9. customyielding
  10. customwhen dried

出典と根拠

ORDレコード
ord-2fc511b73fdf4e8283cdd24ced3f170e
出典データセット
uspto-grants-1996_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05587379

反応ノート

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