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1-Hydroxybenzotriazole → HCID 22101906, 화합물

HRID 1458292
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HRID 1458292 반응식
[CH2:1]([O:11][C:12]1[CH:20]=[CH:19][CH:18]=[CH:17][C:13]=1[C:14]([OH:16])=O)/[CH:2]=[C:3](/[CH2:5][CH2:6][CH:7]=[C:8]([CH3:10])[CH3:9])\[CH3:4].ON1C2C=CC=CC=2N=N1.Cl.CN(C)CCCN=C=NCC.[NH2:43][CH:44]1[CH2:48][N:47]([CH2:49][CH3:50])[N:46]([CH2:51][CH3:52])[CH2:45]1>ClCCl>[CH2:51]([N:46]1[CH2:45][CH:44]([NH:43][C:14](=[O:16])[C:13]2[CH:17]=[CH:18][CH:19]=[CH:20][C:12]=2[O:11][CH2:1]/[CH:2]=[C:3](/[CH2:5][CH2:6][CH:7]=[C:8]([CH3:9])[CH3:10])\[CH3:4])[CH2:48][N:47]1[CH2:49][CH3:50])[CH3:52]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 757711-HydroxybenzotriazoleHCID 5591991,2-Diethyl-4-pyrazolidinamineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 53471241HCID 53471241, 화합물

생성물 1

HCID 22101906HCID 22101906, 화합물수율 87%

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매

실험 절차

2-geranyloxybenzoic acid (1.36 g) was dissolved in dichloromethan (20 ml) and 1-hydroxybenzotriazole (0.80 g) and 1-(3-dimethylaminopropyl)-3-ethyl carbodiimide hydrochloride (1.14 g) were added thereto while being cooled with ice. After the resulting mixture was stirred for 30 minutes, 4-amino-1,2-diethyl pyrazolidine (0.71 g) was added thereto and the mixture was stirred for one night at room temperature. The reaction liquid was washed with brine and then dried over sodium sulfite anhydride. Thereafter, the solvent was evaporated under a vacuum. The residue was purified by silica gel column-m chromatography (chloroform:methanol=30:1), thereby yielding 1.71 g (87%) of the aimed compound.

후처리

  1. temperaturewhile being cooled with ice
  2. stirringthe mixture was stirred for one night at room temperature
  3. customThe reaction liquid
  4. washwas washed with brine
  5. dry with materialdried over sodium sulfite anhydride
  6. customThereafter, the solvent was evaporated under a vacuum
  7. customThe residue was purified by silica gel column-m chromatography (chloroform:methanol=30:1)

출처 및 근거

ORD 기록
ord-e99ccb1cacd949e393c4609300a762f7
출처 데이터셋
uspto-grants-1998_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05849930

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