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Ammonium Carbonate → HCID 19389968, 화합물

HRID 1757148
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HRID 1757148 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[C:9]1([C:16](=[O:17])NC(=O)[NH:13]1)[CH2:8][CH2:7][CH2:6]2.O.O.O.O.O.O.O.O.[OH-].[Ba+2].[OH-].C(=O)([O-])[O-:31].[NH4+].[NH4+]>O>[NH2:13][C:9]1([C:16]([OH:17])=[O:31])[C:10]2[C:5](=[CH:4][C:3]([O:2][CH3:1])=[CH:12][CH:11]=2)[CH2:6][CH2:7][CH2:8]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 517111Ammonium CarbonateHCID 29981396'-methoxy-3',4'-dihydro-2'H-spiro[imidazolidine-4,1'-naphthalene]-2,5-dioneHCID 17749109Barium hydroxide, octahydrate

생성물 1

HCID 19389968HCID 19389968, 화합물수율 70.1%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a suspension of 2.95 g (0.012 mol) of the product of Step A in 100 mL of water was added 15.1 g (0.0479 mol) of barium hydroxide octahydrate. The reaction was heated at reflux for 3 days. To the reaction mixture was carefully added 6.4 g (0.067 mol) of ammonium carbonate. Refluxing was continued for another 2 hours. The solid was filtered off while hot and the pH of the filtrate adjusted to 6. The filtrate was then concentrated to give 1.86 g of a tan solid: mp>250° C. 1H NMR (D2O) d 7.20 (d, 1H), 6.85 (d and s, 2H), 3.835 (s, 3H), 2.85 (t, 2H), 1.70-2.40 (m, 4H).

후처리

  1. temperatureThe reaction was heated
  2. temperatureat reflux for 3 days
  3. temperatureRefluxing
  4. filtrationThe solid was filtered off while hot and the pH of the filtrate
  5. concentrationThe filtrate was then concentrated

출처 및 근거

ORD 기록
ord-aa90eb05c4544a6db56d68895c571790
출처 데이터셋
uspto-grants-1995_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05444079

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