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1-ethyl-5-pyrrolidin-1-yl-3-trimethylsilanylethynyl-1H-[1,2,4]triazole → 1-ethyl-3-ethynyl-5-pyrrolidin-1-yl-1H-[1,2,4]triazole

HRID 1054978
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인쇄 미리보기

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HRID 1054978 반응식
[CH2:1]([N:3]1[C:7]([N:8]2[CH2:12][CH2:11][CH2:10][CH2:9]2)=[N:6][C:5]([C:13]#[C:14][Si](C)(C)C)=[N:4]1)[CH3:2]>CO.[OH-].[Na+].C(OCC)(=O)C>[CH2:1]([N:3]1[C:7]([N:8]2[CH2:12][CH2:11][CH2:10][CH2:9]2)=[N:6][C:5]([C:13]#[CH:14])=[N:4]1)[CH3:2]
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참가 물질

5

반응물 1

HCID 900256441-ethyl-5-pyrrolidin-1-yl-3-trimethylsilanylethynyl-1H-[1,2,4]triazole

생성물 1

HCID 900168721-ethyl-3-ethynyl-5-pyrrolidin-1-yl-1H-[1,2,4]triazole수율 89.3%

시약·촉매·용매 3

HCID 887Methanol용매HCID 8857Ethyl Acetate용매HCID 14798Sodium Hydroxide용매

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온도
25 °C

실험 절차

A mixture of 1-ethyl-5-(pyrrolidin-1-yl)-3-((trimethylsilyl)ethynyl)-1H-1,2,4-triazole (122 mg, 465 μmol, Eq: 1.00) in methanol (3 ml) and 1N NaOH aq. (0.1 ml) was stirred for 18 hours at 25° C. under argon atmosphere. The mixture was diluted with ethyl acetate and washed with water. The organic layer was separated, dried over magnesium sulfate, filtered and concentrated affording 1-ethyl-3-ethynyl-5-pyrrolidin-1-yl-1H-[1,2,4]triazole (79 mg, 89.3%) as an orange oil. MS: m/z=191.2 (M+H+)

후처리

  1. washwashed with water
  2. customThe organic layer was separated
  3. dry with materialdried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-0eb44f9ab9f349ebb90191742d90bd9e
출처 데이터셋
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09394311B2

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