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Tetrahydrofuran → HCID 58409914, 화합물

HRID 1844912
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HRID 1844912 반응식
[N:1]1([C:6]2[CH:18]=[C:17]([C:19]3[CH:24]=[CH:23][C:22]([CH3:25])=[CH:21][CH:20]=3)[C:16]3[C:15]4[C:10](=[CH:11][CH:12]=[CH:13][CH:14]=4)[CH2:9][C:8]=3[C:7]=2[C:26]#[N:27])[CH2:5][CH2:4][CH2:3][CH2:2]1.[H-].[Na+].C1C[O:33]CC1>>[O:33]=[C:9]1[C:8]2[C:7]([C:26]#[N:27])=[C:6]([N:1]3[CH2:5][CH2:4][CH2:3][CH2:2]3)[CH:18]=[C:17]([C:19]3[CH:20]=[CH:21][C:22]([CH3:25])=[CH:23][CH:24]=3)[C:16]=2[C:15]2[C:10]1=[CH:11][CH:12]=[CH:13][CH:14]=2
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 8028TetrahydrofuranHCID 24758Sodium hydrideHCID 58409954HCID 58409954, 화합물

생성물 1

HCID 58409914HCID 58409914, 화합물수율 76%

반응 조건

온도
2.5 °C

실험 절차

A solution of 2-(pyrrolidin-1-yl)-4-p-tolyl-9H-fluorene-1-carbonitrile (350 mg) in THF was added sodium hydride (42 mg) and was stirred at 0-5° C. for less than five minutes. After completion, the reaction solvent was evaporated under vacuum and the crude solid obtained was quenched with ice water and subsequently neutralized by dilute HCl. The precipitate thus obtained was filtered and purified on a silica gel column using ethyl acetate-hexane as eluent. Red solid; yield 76%; mp 162-164° C.; ESMS 365 (M++1); IR (KBr) 1716 cm−1 (CO) 2214 (CN).

후처리

  1. customAfter completion, the reaction solvent was evaporated under vacuum
  2. customthe crude solid obtained
  3. customwas quenched with ice water
  4. customThe precipitate thus obtained
  5. filtrationwas filtered
  6. custompurified on a silica gel column

출처 및 근거

ORD 기록
ord-5aa8f16b97d14ca4ad16372ba350cd24
출처 데이터셋
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08946682B2

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