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Water → 5-amino-4-(2-aminoethyl)-1-(2-triphenylmethyloxyethyl)-1H-pyrazole

HRID 349550
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인쇄 미리보기

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HRID 349550 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[NH2:7][C:8]1[N:12]([CH2:13][CH2:14][O:15][C:16]([C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[N:11]=[CH:10][C:9]=1/[CH:35]=[CH:36]/[N+:37]([O-])=O.[F-].[Na+].O>O1CCCC1>[NH2:7][C:8]1[N:12]([CH2:13][CH2:14][O:15][C:16]([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)([C:17]2[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=2)[C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)[N:11]=[CH:10][C:9]=1[CH2:35][CH2:36][NH2:37]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 5235Sodium FluorideHCID 179619895-amino-4-[(E)-2-nitroethenyl]-1-(2-triphenylmethyloxyethyl)-1H-pyrazoleHCID 21226445Aluminium lithium hydride

생성물 1

HCID 179619655-amino-4-(2-aminoethyl)-1-(2-triphenylmethyloxyethyl)-1H-pyrazole수율 88.1%

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매

실험 절차

To a suspension of lithium aluminum hydride (3.22 g) in tetrahydrofuran (100 ml) was added 5-amino-4-[(E)-2-nitroethenyl]-1-(2-triphenylmethyloxyethyl)-1H-pyrazole (4.4 g) under ice-cooling. The mixture was refluxed for 5 hours. After cooling on an ice bath, sodium fluoride (14.3 g) and water (6.12 ml) were added to the reaction mixture. The insoluble materials were removed by filtration. The filtrate was concentrated in vacuo to give 5-amino-4-(2-aminoethyl)-1-(2-triphenylmethyloxyethyl)-1H-pyrazole (3.63 g). This product was used in the next step without further purification.

후처리

  1. temperaturecooling
  2. temperatureThe mixture was refluxed for 5 hours
  3. temperatureAfter cooling on an ice bath
  4. customThe insoluble materials were removed by filtration
  5. concentrationThe filtrate was concentrated in vacuo

출처 및 근거

ORD 기록
ord-f01b71e726264165b778faec246c47c5
출처 데이터셋
uspto-grants-2007_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07179801B2

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