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1-Hydroxybenzotriazole → HCID 22101906、化合物

HRID 1458292
ノート
印刷プレビュー

反応式

HRID 1458292 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

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

生成物 1

HCID 22101906HCID 22101906、化合物収率 87%

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-e99ccb1cacd949e393c4609300a762f7
出典データセット
uspto-grants-1998_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05849930

反応ノート

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