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Hydrochloric Acid → HCID 11075774, 화합물

HRID 725919
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HRID 725919 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][C:11]=1[O:12][CH3:13])[CH2:8][CH:7]([NH2:14])[CH2:6]2.C(=O)([O-])[O-].[Na+].[Na+].Cl>CN(C)C=O.C(#N)C.C(OCC)(=O)C>[CH3:13][O:12][C:11]1[CH:10]=[C:9]2[C:5](=[CH:4][C:3]=1[O:2][CH3:1])[CH2:6][CH:7]([N:14]1[CH2:10][CH2:11][CH2:3][CH2:4]1)[CH2:8]2
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참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 10340Sodium CarbonateHCID 110416235,6-dimethoxy-2,3-dihydro-1H-inden-2-amine

생성물 1

HCID 11075774HCID 11075774, 화합물

시약·촉매·용매 2

HCID 8857Ethyl Acetate용매HCID 21891449acetonitrile N,N-dimethylformamide용매

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온도
100 °C

실험 절차

To a solution of 5,6-dimethoxy-2-aminoindan (Preparation 5, 4.5 mmol) in dimethylformamide/acetonitrile (1:6, 49 mL) was added sodium carbonate (1.43 g, 13.5 mmol) and was heated (100° C.) overnight. The mixture was diluted with ethyl acetate, filtered and the filtrate concentrated. The oily residue was chromatographed (400 g silica gel) eluting with methylene chloride/methanol (9:1) to yield a yellow oil. The oil was converted into the HCl salt and recrystallized from methanol/ethyl acetate: mp 267°-269° C.

후처리

  1. filtrationfiltered
  2. concentrationthe filtrate concentrated
  3. customThe oily residue was chromatographed (400 g silica gel)
  4. washeluting with methylene chloride/methanol (9:1)
  5. customto yield a yellow oil
  6. customrecrystallized from methanol/ethyl acetate

출처 및 근거

ORD 기록
ord-9781a44935ff4ade8a1656b116b13ebb
출처 데이터셋
uspto-grants-1998_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05708018

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