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Ammonium Acetate → HCID 66728926, 화합물

HRID 518775
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HRID 518775 반응식
[NH:1]1[C:5]2([CH2:10][CH2:9][C:8](=O)[CH2:7][CH2:6]2)[C:4](=[O:12])[NH:3][C:2]1=[O:13].C([O-])(=O)C.[NH4+].C([BH3-])#[N:20].[Na+]>CO>[NH2:20][CH:8]1[CH2:9][CH2:10][C:5]2([NH:1][C:2](=[O:13])[NH:3][C:4]2=[O:12])[CH2:6][CH2:7]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 517165Ammonium AcetateHCID 5003444Sodium cyanoborohydrideHCID 667289301,3-Diazaspiro[4.5]decane-2,4,8-trione

생성물 1

HCID 66728926HCID 66728926, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a suspension of 1,3-diazaspiro[4.5]decane-2,4,8-trione (5.00 g, 27.4 mmol) in MeOH (91 mL) was added ammonium acetate (6.35 g, 82 mmol), and the mixture was stirred at RT for 25 minutes. To the suspension was added sodium cyanoborohydride (5.17 g, 82 mmol), and the mixture was stirred at RT. After 90 minutes, the flask was cooled, and the contents were quenched by careful addition of aqueous concentrated HCl, adjusting the pH to 7 with solid NaHCO3. The mixture was filtered through a pad of Celite® brand filter aid and concentrated in vacuo. The material was used directly in the next step.

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후처리

  1. stirringthe mixture was stirred at RT
  2. waitAfter 90 minutes
  3. temperaturethe flask was cooled
  4. customthe contents were quenched by careful addition of aqueous concentrated HCl
  5. filtrationThe mixture was filtered through a pad of Celite® brand
  6. filtrationfilter aid
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-f66643498a854f3982445e41d96a422f
출처 데이터셋
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09115127B2

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