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Water → HCID 178431816、化合物

HRID 1582225
ノート
印刷プレビュー

反応式

HRID 1582225 の反応式
C[O-].[Na+].Cl.[NH2:5][C:6]([NH2:8])=[NH:7].N1C=CC=CC=1.[S:15]([OH:35])([O:18][C:19]1[C:20]([CH3:34])=[C:21]2[C:25](=[CH:26][CH:27]=1)[N:24]([CH3:28])[C:23]([C:29](OCC)=[O:30])=[CH:22]2)(=[O:17])=[O:16].O>CN(C)C=O>[S:15]([OH:35])([O:18][C:19]1[C:20]([CH3:34])=[C:21]2[C:25](=[CH:26][CH:27]=1)[N:24]([CH3:28])[C:23]([C:29]([NH:7][C:6]([NH2:8])=[NH:5])=[O:30])=[CH:22]2)(=[O:16])=[O:17]
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 5742Guanidine HydrochlorideHCID 10942334Sodium MethoxideHCID 22719997HCID 22719997、化合物

生成物 1

HCID 178431816HCID 178431816、化合物収率 82%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

A mixture of sodium methoxide (4.28 g, 79.2 mmol), guanidine hydrochloride (7.58 g, 79.3 mmol) and N,N-dimethylformamide (70 ml) was stirred at room temperature for 1 hour, and then the insoluble material was filtered off. A solution of 2-ethoxycarbonyl-1,4-dimethyl-1H-indole-5-yl hydrogen sulfate pyridine salt (3.11 g, 7.92 mmol) in N,N-dimethylformamide (10 ml) was added to the filtrate, and the resulting mixture was stirred at room temperature for 7.5 hours. Water was added to the reaction mixture, followed by washing with chloroform. Subsequently, chloroform and then 2N hydrochloric acid were added and the solid thus precipitated was collected by filtration and washed with methanol to obtain 2.12 g of 2-[[[amino(imino)-methyl]amino]carbonyl]-1,4-dimethyl-1H-indol-5-yl hydrogen sulfate.

後処理

  1. filtrationthe insoluble material was filtered off
  2. stirringthe resulting mixture was stirred at room temperature for 7.5 hours
  3. washby washing with chloroform
  4. additionSubsequently, chloroform and then 2N hydrochloric acid were added
  5. customthe solid thus precipitated
  6. filtrationwas collected by filtration
  7. washwashed with methanol

出典と根拠

ORDレコード
ord-037b4ad781624dda99ca11115e5c1d23
出典データセット
uspto-grants-2004_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06734205B2

反応ノート

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