HCID 86702385, 화합물 → HCID 86702386, 화합물

HRID 1851245노트

반응식

HRID 1851245 반응식
[NH2:1][C:2]([C:18]1[CH:23]=[CH:22][CH:21]=[C:20]([CH3:24])[N:19]=1)=[N:3][NH:4][C:5]([CH:7]1[CH2:10][N:9]([C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[CH2:8]1)=O>C(O)C>[CH3:24][C:20]1[N:19]=[C:18]([C:2]2[N:1]=[C:5]([CH:7]3[CH2:10][N:9]([C:11]([O:13][C:14]([CH3:17])([CH3:16])[CH3:15])=[O:12])[CH2:8]3)[NH:4][N:3]=2)[CH:23]=[CH:22][CH:21]=1

참가 물질

3

반응물 1

HCID 86702385HCID 86702385, 화합물

생성물 1

HCID 86702386HCID 86702386, 화합물수율 83%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

16.4 g (49.3 mmol) tert-Butyl 3-({2-[amino(6-methylpyridine-2-yl)methylene]hydrazino}carbonyl)azetidine-1-carboxylate are heated under a nitrogen atmosphere to the melting point (220° C.) and kept there for 90 minutes. Ethanol is cautiously added to the reaction mixture during the cooling down phase (at around 135° C.). The reaction mixture is stirred over night at room temperature and the ethanol is evaporated. Due to an incomplete reaction the residue is heated once more to 220° C. for one hour and the work up is repeated yielding 12.91 g (74.58%) of the desired crude product (the byproduct is the cyclised compound which has lost the Boc group).

후처리

  1. customthe ethanol is evaporated
  2. customDue to an incomplete reaction the residue
  3. temperatureis heated once more to 220° C. for one hour

출처 및 근거

ORD 기록
ord-e2320281abda4a90afe668ffba273b47
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08957064B2

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