Methyl iodide → HCID 19756360、化合物

HRID 1587832ノート

反応式

HRID 1587832 の反応式
[H-].[Na+].[CH2:3]([C:5]1[CH:14]=[C:13]([O:15][CH2:16][C:17]2[CH:22]=[CH:21][C:20]([C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=3[C:29]3[N:30]=[N:31][N:32]([C:34]([C:47]4[CH:52]=[CH:51][CH:50]=[CH:49][CH:48]=4)([C:41]4[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=4)[C:35]4[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=4)[N:33]=3)=[CH:19][CH:18]=2)[C:12]2[C:7](=[CH:8][CH:9]=[C:10]([O:53][CH2:54][CH2:55][OH:56])[N:11]=2)[N:6]=1)[CH3:4].[H][H].CI.C1C[O:64][CH2:63][CH2:62]1>O>[CH2:3]([C:5]1[CH:14]=[C:13]([O:15][CH2:16][C:17]2[CH:18]=[CH:19][C:20]([C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=3[C:29]3[N:30]=[N:31][N:32]([C:34]([C:47]4[CH:48]=[CH:49][CH:50]=[CH:51][CH:52]=4)([C:41]4[CH:42]=[CH:43][CH:44]=[CH:45][CH:46]=4)[C:35]4[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=4)[N:33]=3)=[CH:21][CH:22]=2)[C:12]2[C:7](=[CH:8][CH:9]=[C:10]([O:53][CH2:54][C:55]([O:64][CH2:63][CH3:62])=[O:56])[N:11]=2)[N:6]=1)[CH3:4]

参加物

7

反応物 5

HCID 6328Methyl iodideHCID 8028TetrahydrofuranHCID 24758Sodium hydrideHCID 19756350HCID 19756350、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 19756360HCID 19756360、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

Sodium hydride (60% dispersion in mineral oil, 62 mg) was added in a solution of 2-ethyl-6-(2-hydroxyethoxy)-4-[(2'-(2-triphenylmethyl-2H-tetrazol-5-yl)biphenyl-4-yl)methoxy]-1,5-naphthyridine (1.0 g) in THF (10 ml). The mixture was stirred until evolution of hydrogen had ceased and then methyl iodide (0.09 ml) was added. The solution was left to stand for 72 hours and then water (30 ml) was added. The mixture was extracted with ether (2×20 ml) and the combined extracts were dried (MgSO4). Volatile material was removed by evaporation and the residue was triturated with hexane to give 2-ethyl-6-(2-methoxyethoxy)-4-[(2'-(2-triphenylmethyl-2H-tetrazol-5-yl)biphenyl-4-yl)methoxy]-1,5-naphthyridine (A) (0.86 g), as a foam; NMR (d6 -DMSO): 1.3(t, 3H), 2.8(q, 2H), 3.25(s, 3H), 3.6-3.7(m, 2H), 4.45-4.55(m, 2H), 5.4(s, 2H), 6.8-6.9(m, 6H), 7.1-7.7(complex m, 18H), 7.8(dd, 1H), 8.15(d, 1H).

後処理

  1. waitThe solution was left
  2. extractionThe mixture was extracted with ether (2×20 ml)
  3. dry with materialthe combined extracts were dried (MgSO4)
  4. customVolatile material was removed by evaporation
  5. customthe residue was triturated with hexane

出典と根拠

ORDレコード
ord-57fcaaabc29c4f6ab879df9c4106f3c2
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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