Tetrabutylammonium Fluoride → HCID 19756350, 화합물

HRID 1587827노트

반응식

HRID 1587827 반응식
[F-].C([N+](CCCC)(CCCC)CCCC)CCC.[Si]([O:36][CH2:37][CH2:38][O:39][C:40]1[N:41]=[C:42]2[C:47](=[CH:48][CH:49]=1)[N:46]=[C:45]([CH2:50][CH3:51])[CH:44]=[C:43]2[O:52][CH2:53][C:54]1[CH:59]=[CH:58][C:57]([C:60]2[CH:65]=[CH:64][CH:63]=[CH:62][C:61]=2[C:66]2[N:67]=[N:68][N:69]([C:71]([C:84]3[CH:89]=[CH:88][CH:87]=[CH:86][CH:85]=3)([C:78]3[CH:83]=[CH:82][CH:81]=[CH:80][CH:79]=3)[C:72]3[CH:77]=[CH:76][CH:75]=[CH:74][CH:73]=3)[N:70]=2)=[CH:56][CH:55]=1)(C(C)(C)C)(C1C=CC=CC=1)C1C=CC=CC=1>O1CCCC1.C(OCC)(=O)C>[CH2:50]([C:45]1[CH:44]=[C:43]([O:52][CH2:53][C:54]2[CH:55]=[CH:56][C:57]([C:60]3[CH:65]=[CH:64][CH:63]=[CH:62][C:61]=3[C:66]3[N:67]=[N:68][N:69]([C:71]([C:84]4[CH:85]=[CH:86][CH:87]=[CH:88][CH:89]=4)([C:78]4[CH:79]=[CH:80][CH:81]=[CH:82][CH:83]=4)[C:72]4[CH:77]=[CH:76][CH:75]=[CH:74][CH:73]=4)[N:70]=3)=[CH:58][CH:59]=2)[C:42]2[C:47](=[CH:48][CH:49]=[C:40]([O:39][CH2:38][CH2:37][OH:36])[N:41]=2)[N:46]=1)[CH3:51]

참가 물질

5

반응물 2

HCID 2724141Tetrabutylammonium FluorideHCID 53976296HCID 53976296, 화합물

생성물 1

HCID 19756350HCID 19756350, 화합물수율 89.9%

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매2회HCID 8857Ethyl Acetate용매

실험 절차

A 1M solution of tetrabutylammonium fluoride in tetrahydrofuran (THF) (67.8 ml) was added to a solution of compound E (32.1 g) in dry THF (400 ml), and the solution was left to stand for 1 hour. The solution was then diluted with ethyl acetate (400 ml), washed with water (400 ml) and dried (MgSO4). Volatile material was removed by evaporation, and the residue triturated with ether to give 2-ethyl-6-(2-hydroxyethoxy)-4-[(2'-(2-triphenylmethyl-2H-tetrazol-5-yl)biphenyl-4-yl)methoxy]-1,5-naphthyridine (A) (21.6 g), as a white solid, m.p. 170°-173° C.; NMR (d6 -DMSO): 1.3(t,3H), 2.85(q,2H), 3.75(q,2H), 4.45(t,2H), 4.85(t,1H), 5.35(s,2H), 6.8-6.9(m,7H), 7.1-7.7 (complex m,17H), 7.8(dd,1H), 8.15(d,1H).

후처리

  1. waitthe solution was left
  2. washwashed with water (400 ml)
  3. dry with materialdried (MgSO4)
  4. customVolatile material was removed by evaporation
  5. customthe residue triturated with ether

출처 및 근거

ORD 기록
ord-1998c13414f04aca82fe5466a6851935
출처 데이터셋
uspto-grants-1993_06
특허 번호
US05219863

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