9-Fluorenylmethyl carbazate → 5-[N'-(9H-fluoren-9-ylmethoxycarbonyl)hydrazino]-5-oxo-3-phenylpentanoic acid

HRID 480006노트

반응식

HRID 480006 반응식
[C:1]1([CH:7]2[CH2:13][C:12](=[O:14])[O:11][C:9](=[O:10])[CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[C:15]([NH:32][NH2:33])([O:17][CH2:18][CH:19]1[C:31]2[C:26](=[CH:27][CH:28]=[CH:29][CH:30]=2)[C:25]2[C:20]1=[CH:21][CH:22]=[CH:23][CH:24]=2)=[O:16]>C1COCC1>[CH:21]1[C:20]2[CH:19]([CH2:18][O:17][C:15]([NH:32][NH:33][C:12](=[O:14])[CH2:13][CH:7]([C:1]3[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=3)[CH2:8][C:9]([OH:11])=[O:10])=[O:16])[C:31]3[C:26](=[CH:27][CH:28]=[CH:29][CH:30]=3)[C:25]=2[CH:24]=[CH:23][CH:22]=1

참가 물질

4

반응물 2

HCID 1618839-Fluorenylmethyl carbazateHCID 2978824-Phenyloxane-2,6-dione

생성물 1

HCID 106945935-[N'-(9H-fluoren-9-ylmethoxycarbonyl)hydrazino]-5-oxo-3-phenylpentanoic acid

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

2.0 mmol of 3-phenylglutaric anhydride and 2.0 mmol of Fmoc-hydrazine are dissolved in 30 ml of THF and heated under reflux for 16 hours. The product is then extracted with 50 ml of DCM and 50 ml of 1N HCl solution and the organic phase is dried with MgSO4 and filtered off. Removal of the solvent gives 5-[N′-(9H-fluoren-9-ylmethoxycarbonyl)hydrazino]-5-oxo-3-phenylpentanoic acid.

후처리

  1. temperatureheated
  2. temperatureunder reflux for 16 hours
  3. extractionThe product is then extracted with 50 ml of DCM and 50 ml of 1N HCl solution
  4. dry with materialthe organic phase is dried with MgSO4
  5. filtrationfiltered off
  6. customRemoval of the solvent

출처 및 근거

ORD 기록
ord-9cd8bef05875445da19818467726c812
출처 데이터셋
uspto-grants-2003_11
특허 번호
US06649613B1

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