Tetrahydrofuran → HCID 58409925, 화합물

HRID 1844906노트

반응식

HRID 1844906 반응식
[CH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][C:2]=1[C:11]1[C:23]2[C:22]3[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=3)[CH2:16][C:15]=2[C:14]([C:24]#[N:25])=[C:13]([N:26]2[CH2:31][CH2:30][CH2:29][CH2:28][CH2:27]2)[CH:12]=1.[H-].[Na+].C1C[O:37]CC1>>[CH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][C:2]=1[C:11]1[C:23]2[C:22]3[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=3)[C:16](=[O:37])[C:15]=2[C:14]([C:24]#[N:25])=[C:13]([N:26]2[CH2:31][CH2:30][CH2:29][CH2:28][CH2:27]2)[CH:12]=1

참가 물질

4

반응물 3

HCID 8028TetrahydrofuranHCID 24758Sodium hydrideHCID 58409919HCID 58409919, 화합물

생성물 1

HCID 58409925HCID 58409925, 화합물

반응 조건

온도
2.5 °C

실험 절차

A solution of 4-(naphthalen-2-yl)-2-(piperidin-1-yl)-9H-fluorene-1-carbonitrile (400 mg) in THF was added sodium hydride (32 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. Light red solid; mp 182-184° C.; ESIMS 415 (M++1); IR (KBr) 2213 (CN), 1695 cm−1 (CO).

후처리

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

출처 및 근거

ORD 기록
ord-59d70f2d729249828aaa3d2308484666
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08946682B2

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