ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Sodium dicyanamide → HCID 178512346、化合物

HRID 543243
ノート
印刷プレビュー

反応式

HRID 543243 の反応式
Cl.[CH:2]1([NH2:12])[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH2:5][CH2:4][CH2:3]1.[N-:13]([C:16]#[N:17])[C:14]#[N:15].[Na+]>O>[C:14]([NH:13][C:16](=[NH:17])[NH:12][CH:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH2:5][CH2:4][CH2:3]1)#[N:15]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 4350929Sodium dicyanamideHCID 101926091-Naphthylamine, 1,2,3,4-tetrahydro-, hydrochloride

生成物 1

HCID 178512346HCID 178512346、化合物収率 18.1%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A solution of 18.4 grams (g) of 1,2,3,4-tetrahydro-1-naphthylamine hydrochloride and 8.90 g of sodium dicyanamide in 220 milliliters (ml) of water was heated at 95° C. (steam bath) for 21 hours, after which time a viscous oil had precipitated from the hot solution. The reaction mixture was then cooled and extracted with methylene chloride. The methylene chloride extract was dried over anhydrous sodium sulfate and the sodium sulfate removed by filtration. The methylene chloride was then removed by evaporation in vacuo, leaving the crude product as a pale yellow gum. The gum was crystallized from isopropyl acetate to give an off-white, crystalline solid, melting point (mp) 153.5°-156.5° C. Recrystallization from aqueous ethanol gave 3.87 g of N'-cyano-N-(1,2,3,4-tetrahydro-1-naphthyl)guanidine as a white, crystalline solid, mp 157°-158° C.

後処理

  1. customafter which time a viscous oil had precipitated from the hot solution
  2. temperatureThe reaction mixture was then cooled
  3. extractionextracted with methylene chloride
  4. extractionThe methylene chloride extract
  5. dry with materialwas dried over anhydrous sodium sulfate
  6. customthe sodium sulfate removed by filtration
  7. customThe methylene chloride was then removed by evaporation in vacuo
  8. customleaving the crude product as a pale yellow gum
  9. customThe gum was crystallized from isopropyl acetate
  10. customto give an off-white, crystalline solid
  11. custompoint (mp) 153.5°-156.5° C
  12. customRecrystallization from aqueous ethanol

出典と根拠

ORDレコード
ord-63a99f02a1f6486a8beae3ed66d07af4
出典データセット
uspto-grants-1987_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04661520

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