Hydrochloric Acid → 2-Hydroxyimino-N-indan-5-yl-acetamide

HRID 604615

反応式

HRID 604615 の反応式
Cl[C:2](Cl)(Cl)[CH:3]([OH:5])O.[O-]S([O-])(=O)=O.[Na+].[Na+].S(O)(O)(=O)=O.[NH2:20][OH:21].[NH2:22][C:23]1[CH:24]=[C:25]2[C:29](=[CH:30][CH:31]=1)[CH2:28][CH2:27][CH2:26]2.Cl>O>[OH:21][N:20]=[CH:2][C:3]([NH:22][C:23]1[CH:24]=[C:25]2[C:29](=[CH:30][CH:31]=1)[CH2:28][CH2:27][CH2:26]2)=[O:5]

参加物

7

反応物 5

HCID 313Hydrochloric AcidHCID 2707Chloral HydrateHCID 24436Sodium SulfateHCID 90496Indan-5-amineHCID 159255Hydroxylamine, sulfate (1:1)

生成物 1

HCID 722820052-Hydroxyimino-N-indan-5-yl-acetamide

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

反応条件

温度
75 °C

実験手順

To a solution of chloral hydrate (8.34 g, 50.4 mmol) and anhydrous Na2SO4 (43 g, 303 mmol) in water (135 mL) was added a mixture of hydroxylamine sulfate (38.4 g, 234 mmol), 5-aminoindan (6 g, 45 mmol), concentrated HCl (4.71 mL) in water (45 mL). The mixture was heated at 45° C. for 1 h and at 75° C. for 2 h. The reaction mixture was cooled to room temperature. The solid formed was filtered and washed with water. The solid was dried under vacuo to afford 2-hydroxyimino-N-indan-5-yl-acetamide. 1H NMR (500 MHz, DMSO-d6) δ 12.08 (s, 1H); 10.01 (s, 1H); 7.62 (s, 1H); 7.57 (s, 1H); 7.36 (d, J=8.1 Hz, 1H); 7.14 (d, J=8.1 Hz, 1H); 2.83-2.77 (m, 4H); 2.00-1.96 (m, 2H).

後処理

  1. temperatureThe reaction mixture was cooled to room temperature
  2. customThe solid formed
  3. filtrationwas filtered
  4. washwashed with water
  5. customThe solid was dried under vacuo

出典と根拠

ORDレコード
ord-d4fe214d84e74386afb20367d301855a
出典データセット
uspto-grants-2011_03
特許番号
US07910592B2

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