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Acetic Acid → HCID 178419920, 화합물

HRID 652161
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HRID 652161 반응식
COC([N:5]1[CH2:10][CH2:9][CH:8]([C:11]2[C:19]3[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=3)[NH:13][N:12]=2)[CH2:7][CH2:6]1)=N.C(O)(=O)C>O>[NH:5]1[CH2:6][CH2:7][CH:8]([C:11]2[C:19]3[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=3)[NH:13][N:12]=2)[CH2:9][CH2:10]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 176Acetic AcidHCID 1784968134-(1H-indazol-3-yl)piperidine-1-carboximidic acid methyl ester

생성물 1

HCID 178419920HCID 178419920, 화합물수율 46.4%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A solution of 4.7 g of 4-(1H-indazol-3-yl)piperidine-1-carboximidic acid methyl ester and 80% of acetic acid was heated under reflux for 48 hrs. The reaction mixture was cooled and poured into water. The aqueous phase was extracted with ether and then made basic by the slow addition of a 50% aqueous sodium hydroxide solution. A solid separated from the solution. The solid was collected and dried. Recrystallization from ethanol yielded 1.7 g (46%) of product. Concentration of the mother liquors from this and another experiment gave additional product, mp 213°-215° C.

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후처리

  1. temperatureunder reflux for 48 hrs
  2. temperatureThe reaction mixture was cooled
  3. extractionThe aqueous phase was extracted with ether
  4. additionmade basic by the slow addition of a 50% aqueous sodium hydroxide solution
  5. customA solid separated from the solution
  6. customThe solid was collected
  7. customdried
  8. customRecrystallization from ethanol

출처 및 근거

ORD 기록
ord-9070a058386b4cdca359de4c4b7dfba5
출처 데이터셋
uspto-grants-1987_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04670447

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