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HCID 18180220、化合物 → 2-Isopropylcarbonylamino-6-amino-3-(2,3,5-trichlorophenyl)pyrazine

HRID 1358979
ノート
印刷プレビュー

反応式

HRID 1358979 の反応式
[CH:1]([C:4]([NH:6][C:7]1[C:12]([C:13]2[CH:18]=[C:17]([Cl:19])[CH:16]=[C:15]([Cl:20])[C:14]=2[Cl:21])=[N:11][CH:10]=[C:9]([NH:22]C(=O)C)[N:8]=1)=[O:5])([CH3:3])[CH3:2]>C(O)C>[CH:1]([C:4]([NH:6][C:7]1[C:12]([C:13]2[CH:18]=[C:17]([Cl:19])[CH:16]=[C:15]([Cl:20])[C:14]=2[Cl:21])=[N:11][CH:10]=[C:9]([NH2:22])[N:8]=1)=[O:5])([CH3:3])[CH3:2]
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

3

反応物 1

HCID 18180220HCID 18180220、化合物

生成物 1

HCID 181802152-Isopropylcarbonylamino-6-amino-3-(2,3,5-trichlorophenyl)pyrazine

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
55 °C

実験手順

Stannous chloride (0.182 g, 0.0096 mole) was added to the suspension of 2-isopropylcarbonylamino-6-acetamido-3-(2,3,5-trichlorophenyl)pyrazine (0.13 g, 3.24×10−4 mole), in absolute ethanol (6.50 ml) and the resulting mixture stirred at 50-60° C. for 1 hr 20 min. The reaction mixture was cooled and evaporated in vacuo. The residue was extracted with ethylacetate (3×20 ml), washed with water (2×20 ml), dried over anhydrous magnesium sulphate, filtered and the filtrate evaporated in vacuo. The residue was purified by ‘flash chromatography’ using chloroform:methanol, 99:1 as the eluent. Yield 0.046 g (40%), M.p. 105-108° C.

後処理

  1. temperatureThe reaction mixture was cooled
  2. customevaporated in vacuo
  3. extractionThe residue was extracted with ethylacetate (3×20 ml)
  4. washwashed with water (2×20 ml)
  5. dry with materialdried over anhydrous magnesium sulphate
  6. filtrationfiltered
  7. customthe filtrate evaporated in vacuo
  8. customThe residue was purified by ‘flash chromatography’

出典と根拠

ORDレコード
ord-35e81cf6f751401296e0c2fbbab1daa2
出典データセット
uspto-grants-2003_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06599905B2

反応ノート

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