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Ammonium Acetate → HCID 66728926、化合物

HRID 518775
ノート
印刷プレビュー

反応式

HRID 518775 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

HCID 66728926HCID 66728926、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  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

出典と根拠

ORDレコード
ord-f66643498a854f3982445e41d96a422f
出典データセット
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09115127B2

反応ノート

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