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Triethylamine → HCID 86702333、化合物

HRID 2279079
ノート
印刷プレビュー

反応式

HRID 2279079 の反応式
C(N(CC)CC)C.Cl[C:9]1[C:14]([N+:15]([O-:17])=[O:16])=[CH:13][CH:12]=[C:11]([Cl:18])[N:10]=1.[Cl:19][C:20]1[CH:21]=[C:22]([NH2:28])[C:23]([O:26][CH3:27])=[N:24][CH:25]=1>C(#N)C>[Cl:18][C:11]1[N:10]=[C:9]([NH:28][C:22]2[C:23]([O:26][CH3:27])=[N:24][CH:25]=[C:20]([Cl:19])[CH:21]=2)[C:14]([N+:15]([O-:17])=[O:16])=[CH:13][CH:12]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 852392,6-Dichloro-3-nitropyridineHCID 451221815-Chloro-2-methoxypyridin-3-amine

生成物 1

HCID 86702333HCID 86702333、化合物収率 39.2%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
90 °C

実験手順

Triethylamine (2.7 mL) and a catalytic amount of 4-diaminopyrimidine were added to a solution of 2,6-dichloro-3-nitropyridine (639 mg, 3.31 mmol) and 5-chloro-2-methoxy pyridin-3-amine (Preparation 23, 501 mg, 3.16 mmol) in acetonitrile (20 mL) and the resulting mixture was stirred overnight at 90° C. Solvent was then removed under reduced pressure until a solid precipitated. The solid was filtered, washed with acetonitrile and dried. The solid was then treated with dichloromethane, filtered, washed with more dichloromethane and the combined filtrate and washings were concentrated to dryness under reduced pressure to yield the title compound (390 mg 30%) as an orange solid.

後処理

  1. customSolvent was then removed under reduced pressure until a solid
  2. customprecipitated
  3. filtrationThe solid was filtered
  4. washwashed with acetonitrile
  5. customdried
  6. additionThe solid was then treated with dichloromethane
  7. filtrationfiltered
  8. washwashed with more dichloromethane
  9. concentrationthe combined filtrate and washings were concentrated to dryness under reduced pressure

出典と根拠

ORDレコード
ord-f2e83d4dc01c42449d4561a80ba1b238
出典データセット
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09133200B2

反応ノート

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