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3-Amino-4-methylbenzohydrazide → HCID 68289152, 화합물

HRID 541418
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HRID 541418 반응식
CO[C:3]1[CH2:4][CH:5]([C:9]2[CH:16]=[CH:15][C:12]([C:13]#[N:14])=[CH:11][CH:10]=2)[CH2:6][CH2:7][N:8]=1.[NH2:17][C:18]1[CH:19]=[C:20]([CH:25]=[CH:26][C:27]=1[CH3:28])[C:21]([NH:23][NH2:24])=O>ClC1C=CC=CC=1Cl>[NH2:17][C:18]1[CH:19]=[C:20]([C:21]2[N:8]3[CH2:7][CH2:6][CH:5]([C:9]4[CH:16]=[CH:15][C:12]([C:13]#[N:14])=[CH:11][CH:10]=4)[CH2:4][C:3]3=[N:24][N:23]=2)[CH:25]=[CH:26][C:27]=1[CH3:28]
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참가 물질

4

반응물 2

HCID 185260563-Amino-4-methylbenzohydrazide2회HCID 68289109HCID 68289109, 화합물2회

생성물 1

HCID 68289152HCID 68289152, 화합물수율 31.2%

시약·촉매·용매 1

HCID 72391,2-Dichlorobenzene용매

반응 조건

온도
150 °C

실험 절차

To a solution of 4-(6-methoxy-2,3,4,5-tetrahydropyridin-4-yl)benzonitrile (compound 347.3, 5.00 g, 23.36 mmol, 1.00 equiv) in 1,2-dichlorobenzene (100 mL) was added 3-amino-4-methylbenzohydrazide (compound 347.4, 4.63 g, 28.0 mmol, 1.20 equiv). The resulting solution was stirred overnight at 150° C. in an oil bath. After cooling to ambient temperature, the resulting mixture was purified using silica gel column chromatography with dichloromethane/methanol (1:0˜100:1) as eluent to furnish 2.40 g (31%) of the title compound as a white solid.

후처리

  1. temperatureAfter cooling to ambient temperature
  2. customthe resulting mixture was purified

출처 및 근거

ORD 기록
ord-43d5a2cfea374db9918d08cf41ca8fb8
출처 데이터셋
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08871790B2

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