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Diisopropylethylamine → HCID 86635093、化合物

HRID 1696200
ノート
印刷プレビュー

反応式

HRID 1696200 の反応式
Cl[C:2]1[CH:7]=[CH:6][N:5]=[C:4]([NH2:8])[C:3]=1[N+:9]([O-:11])=[O:10].Cl.[CH3:13][C@@H:14]1[CH2:19][CH2:18][CH2:17][CH2:16][C@@H:15]1[NH2:20].[CH:21](N(CC)C(C)C)(C)C>CC(O)C>[CH3:21][N:20]([C@H:15]1[CH2:16][CH2:17][CH2:18][CH2:19][C@H:14]1[CH3:13])[C:2]1[CH:7]=[CH:6][N:5]=[C:4]([NH2:8])[C:3]=1[N+:9]([O-:11])=[O:10]
参加物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 81531DiisopropylethylamineHCID 40716944-Chloro-3-nitropyridin-2-amineHCID 672780792-Methylcyclohexylamine hydrochloride, (1S,2R)-

生成物 1

HCID 86635093HCID 86635093、化合物

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

In a microwave reaction vessel 4-chloro-3-nitro-2-pyridinamine (70 mg) and (1S,2R)-2-methylcyclohexanamine hydrochloride (66 mg) were suspended in 2-propanol (0.35 mL). To the mixture was added N,N-diisopropylethylamine (0.21 mL). The vessel was sealed and reacted in the microwave reactor at 130° C. for 1hour. The reaction mixture was concentrated under reduced pressure. The residue was purified by column chromatography on silica gel with chloroform and methanol (100:0 to 90:10) to give N4-methyl-N4-[(1S,2R)-2-methylcyclohexyl]-3-nitro-2,4-pyridinediamine (75 mg) as a yellow amorphous.

後処理

  1. customThe vessel was sealed
  2. customreacted in the microwave reactor at 130° C. for 1hour
  3. concentrationThe reaction mixture was concentrated under reduced pressure
  4. customThe residue was purified by column chromatography on silica gel with chloroform and methanol (100:0 to 90:10)

出典と根拠

ORDレコード
ord-a7947375685944a28bf6bb43aaa39647
出典データセット
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08163767B2

反応ノート

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