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Ammonia → HCID 20393008、化合物

HRID 1862989
ノート
印刷プレビュー

反応式

HRID 1862989 の反応式
[NH2:1][C:2]1[CH:7]=[C:6]([O:8][CH:9]([CH3:11])[CH3:10])[C:5]([O:12][CH:13]([CH3:15])[CH3:14])=[CH:4][C:3]=1[NH2:16].[N:17]#[C:18]Br.N.C(Cl)(Cl)Cl>CO.O>[NH2:17][C:18]1[NH:16][C:3]2[CH:4]=[C:5]([O:12][CH:13]([CH3:15])[CH3:14])[C:6]([O:8][CH:9]([CH3:11])[CH3:10])=[CH:7][C:2]=2[N:1]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 222AmmoniaHCID 6212ChloroformHCID 10476Cyanogen BromideHCID 132301804,5-Bis[(propan-2-yl)oxy]benzene-1,2-diamine

生成物 1

HCID 20393008HCID 20393008、化合物

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962
Water
溶媒
2 回

実験手順

A solution of 1,2-diamino-4,5-di-isopropoxybenzene (2.24 g.) in methanol (40 ml.) was added to a mixture of cyanogen bromide (1.6 g.) in water (40 ml.). The mixture was stirred at 20°-25° C. for 70 hours and then basified by addition of an excess of aqueous ammonia solution (density 0.88). The mixture was then separated by filtration and the filtrate evaporated. The residue which was obtained was mixed with water (50 ml.) and chloroform (50 ml.). The chloroform phase was separated, dried (MgSO4) and evaporated. The residual gum obtained, was purified by chromatography on a column of silica gel (40 g.) using methanol-chloroform (1:3 v/v) as eluant, to give 2-amino-5,6-di-isopropoxybenzimidazole as a sticky solid (1.2 g.), having characteristic absorption bands at ν 3400, 3320, 3080, 1660 and 1565 cm-1, in the infra-red (IR) spectrum.

後処理

  1. customThe mixture was then separated by filtration
  2. customthe filtrate evaporated
  3. customThe residue which was obtained
  4. customThe chloroform phase was separated
  5. dry with materialdried (MgSO4)
  6. customevaporated
  7. customThe residual gum obtained
  8. customwas purified by chromatography on a column of silica gel (40 g.)

出典と根拠

ORDレコード
ord-74b706814d4e47a1a40de4a7bb6596e8
出典データセット
uspto-grants-1979_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04167569

反応ノート

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