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Hydrazine hydrate (1:1) → HCID 11620054, 화합물

HRID 1158181
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HRID 1158181 반응식
[C:1]([C:5]1[CH:6]=[C:7]([C:16]2[CH:17]=[C:18]([C:36]3[CH:41]=[CH:40][C:39]([C:42]([O:44][CH2:45][CH3:46])=[O:43])=[CH:38][CH:37]=3)[CH:19]=[CH:20][C:21]=2[CH2:22][CH2:23][CH2:24][N:25]2C(=O)C3C(=CC=CC=3)C2=O)[CH:8]=[CH:9][C:10]=1[N:11]([CH2:14][CH3:15])[CH2:12][CH3:13])([CH3:4])([CH3:3])[CH3:2].O.NN>C(O)C>[C:1]([C:5]1[CH:6]=[C:7]([C:16]2[CH:17]=[C:18]([C:36]3[CH:41]=[CH:40][C:39]([C:42]([O:44][CH2:45][CH3:46])=[O:43])=[CH:38][CH:37]=3)[CH:19]=[CH:20][C:21]=2[CH2:22][CH2:23][CH2:24][NH2:25])[CH:8]=[CH:9][C:10]=1[N:11]([CH2:14][CH3:15])[CH2:12][CH3:13])([CH3:3])([CH3:4])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 66672038HCID 66672038, 화합물

생성물 1

HCID 11620054HCID 11620054, 화합물수율 77%

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

In a 50 mL three-necked flask under a nitrogen atmosphere, equipped with a magnetic stirrer, 900 mg (1.46 mmol) of ethyl 3″-tert-butyl-4″-diethylamino-4′-[3-(1,3-dioxo-1,3-dihydroisoindol-2-yl)propyl]-[1,1′;3′,1″]terphenyl-4-carboxylate and 292 mg (5.8 mmol) of hydrazine hydrate are placed in 20 mL of ethanol. The reaction medium is heated to the reflux point of the ethanol for 20 hours and then filtered; the filtrate obtained is evaporated and then purified directly on a column of silica (eluent: 94/6 dichloromethane/methanol) to give, after evaporation of the purest fractions, 545 mg of ethyl 3″-tert-butyl-4′-(3-aminopropyl)-4″-diethylamino[1,1′;3′,1″]terphenyl-4-carboxylate (yield=77%) in the form of a colorless oil.

후처리

  1. customIn a 50 mL three-necked flask under a nitrogen atmosphere, equipped with a magnetic stirrer
  2. filtrationfiltered
  3. customthe filtrate obtained
  4. customis evaporated
  5. custompurified directly on a column of silica (eluent: 94/6 dichloromethane/methanol)
  6. customto give

출처 및 근거

ORD 기록
ord-4cf16eb3632f4645a1d3861d4ff57a01
출처 데이터셋
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07807708B2

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