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Sodium Carbonate → HCID 22266170、化合物

HRID 489601
ノート
印刷プレビュー

反応式

HRID 489601 の反応式
[NH2:1][CH2:2][C:3]1[CH:4]=[C:5]([C:9]2([C:22]#[N:23])[CH2:14][CH2:13][N:12]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[CH2:11][CH2:10]2)[CH:6]=[CH:7][CH:8]=1.[C:24](=[O:27])([O-])[O-:25].[Na+].[Na+]>ClCCl.C(N(CC)CC)C.ClC(OCC1C=CC=CC=1)=O>[CH2:2]([O:25][C:24]([NH:1][CH2:2][C:3]1[CH:4]=[C:5]([C:9]2([C:22]#[N:23])[CH2:10][CH2:11][N:12]([C:15]([O:17][C:18]([CH3:19])([CH3:20])[CH3:21])=[O:16])[CH2:13][CH2:14]2)[CH:6]=[CH:7][CH:8]=1)=[O:27])[C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][CH:8]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 2

HCID 10340Sodium CarbonateHCID 22265958HCID 22265958、化合物

生成物 1

HCID 22266170HCID 22266170、化合物

試薬・触媒・溶媒 3

HCID 8471Triethylamine触媒HCID 10387Benzyl chloroformate触媒HCID 6344Dichloromethane溶媒

実験手順

To a solution of 0.2 g of 4-(3-Aminomethyl-phenyl)-1-tert-butoxycarbonyl-piperidine-4-carbonitrile in 15 ml of dichloromethane was added a few drops of triethylamine followed by a few drops of benzyl chloroformate. The mixture was stirred for 1 hour at room temperature and was poured into aqueous sodium carbonate and was extracted with dichloromethane. The organic layer was dried over magnesium sulfate and was filtered. The filtrate was evaporated and the residue was used directly in the next step without further purification: 1H-NMR (300 MHz, CDCl3)δ (TMS) 1.39-1.52 (m, 9H), 1.80-2.16(m, 4H), 3.08-3.42(m, 4H), 4.19-4.50(m, 2H), 5.08-5.13(d, 2H), 7.28-7.79(m, 9H), MS (ESI) m/e 450 (M+H)+.

後処理

  1. extractionwas extracted with dichloromethane
  2. dry with materialThe organic layer was dried over magnesium sulfate
  3. filtrationwas filtered
  4. customThe filtrate was evaporated
  5. customthe residue was used directly in the next step without further purification

出典と根拠

ORDレコード
ord-44520455fadf4012978189d6a47e4642
出典データセット
uspto-grants-2005_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06977263B2

反応ノート

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