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N-Acetyl-4-piperidone → HCID 178473837、化合物

HRID 707332
ノート
印刷プレビュー

反応式

HRID 707332 の反応式
[C:1]([O:5][C:6](=[O:22])[NH:7][C@H:8]1[CH2:11][C@H:10]([N:12]2[C:16]3=[N:17][CH:18]=[CH:19][CH:20]=[C:15]3[C:14]([NH2:21])=[N:13]2)[CH2:9]1)([CH3:4])([CH3:3])[CH3:2].[C:23]([N:26]1[CH2:31][CH2:30][C:29](=O)[CH2:28][CH2:27]1)(=[O:25])[CH3:24].C([BH3-])#N.[Na+].C(=O)(O)[O-].[Na+]>CO.C(O)(=O)C.C(OCC)(=O)C.O>[C:1]([O:5][C:6](=[O:22])[NH:7][C@H:8]1[CH2:11][C@H:10]([N:12]2[C:16]3=[N:17][CH:18]=[CH:19][CH:20]=[C:15]3[C:14]([NH:21][CH:29]3[CH2:30][CH2:31][N:26]([C:23](=[O:25])[CH3:24])[CH2:27][CH2:28]3)=[N:13]2)[CH2:9]1)([CH3:4])([CH3:2])[CH3:3]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

9

反応物 4

HCID 122563N-Acetyl-4-piperidoneHCID 516892Sodium BicarbonateHCID 5003444Sodium cyanoborohydrideHCID 178454109HCID 178454109、化合物

生成物 1

HCID 178473837HCID 178473837、化合物収率 45.2%

試薬・触媒・溶媒 4

HCID 176Acetic Acid
触媒
HCID 887Methanol溶媒
HCID 962Water溶媒
HCID 8857Ethyl Acetate溶媒

反応条件

温度
60 °C

実験手順

Tert-butyl(trans-3-(3-amino-1H-pyrazolo[3,4-b]pyridin-1-yl)cyclobutyl)carbamate (from example 113, step 2, 0.210 g, 0.692 mmol) was dissolved in methanol (4 mL) and acetic acid (3 drops). 1-Acetyl-4-piperidone (0.100 ml, 0.812 mmol) was added and the mixture heated at 60° C. for 1 hour. The solution was cooled and sodium cyanoborohydride (0.065 g, 1.034 mmol) was added. The reaction was stirred for 14 hours at room temperature. Saturated sodium bicarbonate (10 mL), water (50 mL) and ethyl acetate (100 mL) were added and the mixture stirred for 20 minutes. The phases were separated and the organic dried with magnesium sulfate before evaporating to dryness under reduced pressure. Purification using silica chromatography (0-10% methanol in dichloromethane gradient) gave the desired tert-butyl(trans-3-(3-((1-acetylpiperidin-4-yl)amino)-1H-pyrazolo[3,4-b]pyridin-1-yl)cyclobutyl)carbamate (0.134 g, 0.313 mmol, 45.2% yield).

後処理

  1. temperatureThe solution was cooled
  2. stirringthe mixture stirred for 20 minutes
  3. customThe phases were separated
  4. dry with materialthe organic dried with magnesium sulfate
  5. custombefore evaporating to dryness under reduced pressure
  6. customPurification

出典と根拠

ORDレコード
ord-6a3870f68e604a28bbb5b3c672efdf2b
出典データセット
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09174992B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート