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Sodium Carbonate → HCID 22266170, 화합물

HRID 489601
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HRID 489601 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 2

HCID 10340Sodium CarbonateHCID 22265958HCID 22265958, 화합물

생성물 1

HCID 22266170HCID 22266170, 화합물

시약·촉매·용매 3

HCID 8471Triethylamine촉매HCID 10387Benzyl chloroformate촉매HCID 6344Dichloromethane용매

실험 절차

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)+.

후처리

  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

출처 및 근거

ORD 기록
ord-44520455fadf4012978189d6a47e4642
출처 데이터셋
uspto-grants-2005_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06977263B2

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