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Sodium Bicarbonate → HCID 21712328, 화합물

HRID 650841
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HRID 650841 반응식
[CH2:1]([N:8]([C:17]([NH:19][CH2:20][CH3:21])=[O:18])[NH:9]C(OC(C)(C)C)=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(=O)(O)[O-].[Na+]>FC(F)(F)C(O)=O.ClCCl>[CH2:1]([N:8]([C:17]([NH:19][CH2:20][CH3:21])=[O:18])[NH2:9])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 516892Sodium BicarbonateHCID 21712326HCID 21712326, 화합물

생성물 1

HCID 21712328HCID 21712328, 화합물수율 91.6%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 6422Trifluoroacetic acid용매

실험 절차

A solution of of 2-benzyl-1-tert-butoxycarbonyl-4-ethylsemicarbazide (2.8 g, 9.6 mmol) in 50% trifluoroacetic acid in dichloromethane (10 ml) was stirred for 10 min at room temperature. Then saturated sodium bicarbonate was added until pH>7 and the aqueous layer was extracted with dichloromethane (2×10 ml) and the combined organic layers were dried (magnesium sulfate) and concentrated in vacuo. The obtained oil was chromatographed on silica (100 g) with ethyl acetate as eluent to give 1.7 g of 2-benzyl-4-ethylsemicarbazide.

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후처리

  1. extractionthe aqueous layer was extracted with dichloromethane (2×10 ml)
  2. dry with materialthe combined organic layers were dried (magnesium sulfate)
  3. concentrationconcentrated in vacuo
  4. customThe obtained oil was chromatographed on silica (100 g) with ethyl acetate as eluent

출처 및 근거

ORD 기록
ord-06e3f15576a048b9b38f9578fc6d26a8
출처 데이터셋
uspto-grants-2001_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06274584B1

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