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Diethanolamine → HCID 10224851, 화합물

HRID 1797282
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HRID 1797282 반응식
C(N(C(C)C)C(C)C)C.[NH:10]([CH2:14][CH2:15][OH:16])[CH2:11][CH2:12][OH:13].Br[CH2:18]/[CH:19]=[CH:20]/[Sn:21]([CH2:30][CH2:31][CH2:32][CH3:33])([CH2:26][CH2:27][CH2:28][CH3:29])[CH2:22][CH2:23][CH2:24][CH3:25]>CN(C=O)C>[CH2:30]([Sn:21]([CH2:26][CH2:27][CH2:28][CH3:29])([CH2:22][CH2:23][CH2:24][CH3:25])/[CH:20]=[CH:19]/[CH2:18][N:10]([CH2:14][CH2:15][OH:16])[CH2:11][CH2:12][OH:13])[CH2:31][CH2:32][CH3:33]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8113DiethanolamineHCID 81531DiisopropylethylamineHCID 10905679167288-95-1

생성물 1

HCID 10224851HCID 10224851, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
20 °C

실험 절차

N-Ethyl-N,N-diisopropylamine (315 mg) was added to a solution of diethanolamine (256 mg) in dry DMF (5 mL) at 0° C. [(1E)-3-bromoprop-1-enyl](tributyl)stannane (600 mg) was added to the reaction after 10 min. The reaction mixture was stirred for 15 h at 20° C. and then quenched with saturated NH4Cl (aq.). Extraction with Et2O and drying (MgSO4) of the organic phase gave, after concentration in vacuo, the crude product. Purification was done by chromatography eluting with Et2O/MeOH 100:4 to afford the title compound as a liquid.

후처리

  1. additionwas added to the reaction after 10 min
  2. customquenched with saturated NH4Cl (aq.)
  3. extractionExtraction with Et2O
  4. dry with materialdrying (MgSO4) of the organic phase
  5. customgave
  6. concentrationafter concentration in vacuo
  7. customPurification
  8. washeluting with Et2O/MeOH 100:4

출처 및 근거

ORD 기록
ord-0d3e1ae87f7b4061b142c37b49bf6696
출처 데이터셋
uspto-grants-2006_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07034015B2

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