Tetrabutylammonium Fluoride → HCID 19756350、化合物

HRID 1587827ノート

反応式

HRID 1587827 の反応式
[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]

参加物

5

反応物 2

HCID 2724141Tetrabutylammonium FluorideHCID 53976296HCID 53976296、化合物

生成物 1

HCID 19756350HCID 19756350、化合物収率 89.9%

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒2 回HCID 8857Ethyl Acetate溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-1998c13414f04aca82fe5466a6851935
出典データセット
uspto-grants-1993_06
特許番号
US05219863

反応ノート

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