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2-Methoxyethanol → HCID 178496154, 화합물

HRID 1951294
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HRID 1951294 반응식
[CH3:1][O:2][CH2:3][CH2:4][OH:5].[NH2:6][C:7]1[CH:11]=[C:10](O)[NH:9][N:8]=1.C(C=P(CCCC)(CCCC)CCCC)#N>C1C=CC=CC=1>[CH3:1][O:2][CH2:3][CH2:4][O:5][C:10]1[NH:9][N:8]=[C:7]([NH2:6])[CH:11]=1
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참가 물질

5

반응물 3

HCID 80192-MethoxyethanolHCID 962213-Amino-5-hydroxypyrazoleHCID 4622928Cyanomethylenetributylphosphorane

생성물 1

HCID 178496154HCID 178496154, 화합물

시약·촉매·용매 1

HCID 241Benzene용매

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온도
90 °C

실험 절차

To a mixture of 2-methoxyethanol (0.664 mL, 8.41 mmol) and 3-amino-5-hydroxypyrazole (1.00 g, 10.1 mmol) in C6H6 (50 mL) at RT was added cyanomethylenetri-n-butylphosphorane (2.03 g, 8.41 mmol). The mixture was heated to 90° C. in a pressure vessel. After 16 hrs, the solvent was removed in vacuo. The residue was taken up in CH2Cl2 and adsorbed onto silica gel prior to purification by silica gel chromatography using 2-10% MeOH in CH2Cl2 with 1% NH4OH to afford 5-(2-methoxyethoxy)-1H-pyrazol-3-amine as a yellow oil. MH+=158.2.

후처리

  1. customthe solvent was removed in vacuo
  2. customto purification by silica gel chromatography

출처 및 근거

ORD 기록
ord-d104ebc6b4ca4e4babdb55d8f29d1b5d
출처 데이터셋
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08404694B2

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