Hydrochloric Acid → HCID 72740628、化合物

HRID 507063

反応式

HRID 507063 の反応式
Cl[C:2](Cl)(Cl)[CH:3]([OH:5])O.S([O-])([O-])(=O)=O.[Na+].[Na+].S(O)(O)(=O)=O.[NH2:20][OH:21].[NH2:22][C:23]1[CH:31]=[CH:30][CH:29]=[C:28]2[C:24]=1[CH2:25][CH2:26][CH2:27]2.Cl>O>[OH:21][N:20]=[CH:2][C:3]([NH:22][C:23]1[CH:31]=[CH:30][CH:29]=[C:28]2[C:24]=1[CH2:25][CH2:26][CH2:27]2)=[O:5]

参加物

7

反応物 5

HCID 313Hydrochloric AcidHCID 2707Chloral HydrateHCID 24436Sodium SulfateHCID 1225694-AminoindanHCID 159255Hydroxylamine, sulfate (1:1)

生成物 1

HCID 72740628HCID 72740628、化合物収率 90.4%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

反応条件

温度
45 °C

実験手順

To a solution of chloral hydrate (5.46 g, 33 mmol) and anhydrous sodium sulfate (25.6 g, 180 mmol) in water (92 mL) add a mixture of hydroxylamine sulfate (25.6 g, 156 mmol), 4-aminoindane (4 g, 30 mmol), concentrated hydrochloric acid (3.1 mL) in water (30.8 mL). Heat the mixture up to 45° C. for 90 min, to 52° C. over 45 min and to 75° C. for 60 min. Cool the mixture to room temperature and filter the solid. Wash the solid with water and hexane. Dry the solid under vacuum to yield the title compound (5.54 g, 90%). MS (ES−): 203 (M−H).

後処理

  1. waitto 75° C. for 60 min
  2. temperatureCool the mixture to room temperature
  3. filtrationfilter the solid
  4. washWash the solid with water and hexane
  5. customDry the solid under vacuum

出典と根拠

ORDレコード
ord-5698eb4ae42646b0a98745a51caaad1c
出典データセット
uspto-grants-2010_08
特許番号
US07786108B2

関連ノート

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