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Hydrazine hydrate (1:1) → HCID 57834058, 화합물

HRID 730028
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HRID 730028 반응식
[C:1]1([CH:11]([N:13]2C(=O)C3C(=CC=CC=3)C2=O)[CH3:12])[C:10]2[C:4]([CH:5]=[CH:6][CH:7]=[CH:8][CH:9]=2)=[CH:3][CH:2]=1.O.NN>C(O)C>[C:1]1([CH:11]([NH2:13])[CH3:12])[C:10]2[C:4]([CH:5]=[CH:6][CH:7]=[CH:8][CH:9]=2)=[CH:3][CH:2]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 68814169HCID 68814169, 화합물

생성물 1

HCID 57834058HCID 57834058, 화합물수율 97%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
30 °C

실험 절차

2-[1-(Azulen-1-yl)ethyl]-isoindole-1,3-dione (16.8 g) prepared in Example 72, Step B was dissolved in ethanol (400 mL), added with hydrazine monohydrate (3.1 g, Wako Pure Chemical Industries), and stirred at 30° C. for 72 hours. The solid was removed by filtration, and the filtrate was concentrated under reduced pressure. The residue was added with saturated aqueous sodium hydrogencarbonate, and extracted with chloroform. The organic layer was dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by NH silica gel chromatography (NH-DM1020, Fuji Silysia, hexane:ethyl acetate=3:1-1:1) to obtain 9.26 g of the title compound.

후처리

  1. customThe solid was removed by filtration
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. additionThe residue was added with saturated aqueous sodium hydrogencarbonate
  4. extractionextracted with chloroform
  5. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  6. customthe solvent was evaporated under reduced pressure
  7. customThe residue was purified by NH silica gel chromatography (NH-DM1020, Fuji Silysia, hexane:ethyl acetate=3:1-1:1)

출처 및 근거

ORD 기록
ord-a8a211bc0b134580a4b29348545f38b7
출처 데이터셋
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07582658B2

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