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Water → HCID 71295198, 화합물

HRID 527199
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HRID 527199 반응식
[F:1][C:2]1[CH:3]=[C:4]([NH:22][C:23](=O)[O:24]C2C=CC=CC=2)[CH:5]=[CH:6][C:7]=1[N:8]1[CH2:13][CH2:12][N:11]([C:14]2[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=2)[CH2:10][CH2:9]1.[H-].[NH2:33][NH2:34].O>O1CCOCC1>[F:1][C:2]1[CH:3]=[C:4]([NH:22][C:23]([NH:33][NH2:34])=[O:24])[CH:5]=[CH:6][C:7]=1[N:8]1[CH2:13][CH2:12][N:11]([C:14]2[CH:15]=[CH:16][C:17]([O:20][CH3:21])=[CH:18][CH:19]=2)[CH2:10][CH2:9]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 86602801Hydrazine monohydrideHCID 90323117HCID 90323117, 화합물

생성물 1

HCID 71295198HCID 71295198, 화합물수율 82%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

To a solution containing 5 (0.3 g, 0.7 mmol) and hydrazine monohydride (0.19 mL, 3.7 mmol) in 1,4-dioxane. The reaction mixture was stirred and heated to reflux for 4 h. After cooling to room temperature water was added and the mixture was stirred for 30 min. The precipitated solid was filtered and the solid was washed with acetonitrile and then dried under vacuum to obtain the hydrazinecarboxamide intermediate 6 (0.2 g, 82%).

후처리

  1. temperatureheated
  2. temperatureto reflux for 4 h
  3. additionwas added
  4. stirringthe mixture was stirred for 30 min
  5. filtrationThe precipitated solid was filtered
  6. washthe solid was washed with acetonitrile
  7. customdried under vacuum

출처 및 근거

ORD 기록
ord-3fc3f4fa951947ae8f30f2e8137372e1
출처 데이터셋
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09346791B2

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