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

HRID 480006ノート

反応式

HRID 480006 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-9cd8bef05875445da19818467726c812
出典データセット
uspto-grants-2003_11
特許番号
US06649613B1

反応ノート

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