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Hydrazine hydrate (1:1) → HCID 178478013, 화합물

HRID 1376317
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반응식

HRID 1376317 반응식
O.[NH2:2]N.[Cl:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[C:11](=O)[CH:12]=[CH:13][N:14](C)C>C(O)C>[Cl:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[C:11]1[CH:12]=[CH:13][NH:14][N:2]=1
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참가 물질

4

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 538407941-(2-Chlorophenyl)-3-(dimethylamino)prop-2-en-1-one

생성물 1

HCID 178478013HCID 178478013, 화합물수율 77.2%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

7 g (0.0540 mol) of hydrazine hydrate are added, slowly and at room temperature, to a solution of 10.5 g (0.050 mol) of 1-(2-chlorophenyl)-3-dimethylamino-2-propen-1-one, prepared in Example 1, in 60 ml of ethanol. The reaction mixture is stirred for 5 hours at room temperature then left standing for 12 hours before being concentrated to dryness. The residue is recrystallised from a heptane/ethyl acetate mixture. 6.9 g (0.0386 mol) of 3-(2'-chlorophenyl)-1H-pyrazole are obtained, which melts at 93° C. (yield 77%) (compound 60).

후처리

  1. waitthen left
  2. waitstanding for 12 hours
  3. concentrationbefore being concentrated to dryness
  4. customThe residue is recrystallised from a heptane/ethyl acetate mixture

출처 및 근거

ORD 기록
ord-6bcb82e96a524dd69287af115bc387a7
출처 데이터셋
uspto-grants-1997_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05663119

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