Hydrochloric Acid → HCID 72740628, 화합물

HRID 507063

반응식

HRID 507063 반응식
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]

참가 물질

7

반응물 5

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

생성물 1

HCID 72740628HCID 72740628, 화합물수율 90.4%

시약·촉매·용매 1

HCID 962Water용매2회

반응 조건

온도
45 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-5698eb4ae42646b0a98745a51caaad1c
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07786108B2

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