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Sodium Hydroxide → HCID 9809899、化合物

HRID 411289
ノート
印刷プレビュー

反応式

HRID 411289 の反応式
[CH2:1]([N:13]([C:15]([CH2:17][N:18]1[CH:23]=[C:22]([CH2:24][C:25]2[CH:26]=[N:27][C:28](=[O:37])[N:29]([CH2:31][C:32]([O:34]CC)=[O:33])[CH:30]=2)[C:21](=[O:38])[N:20]=[C:19]1[S:39][CH2:40][C:41]1[CH:46]=[CH:45][C:44]([F:47])=[CH:43][CH:42]=1)=[O:16])[CH3:14])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12].[OH-].[Na+]>O1CCOCC1.O>[CH2:1]([N:13]([C:15]([CH2:17][N:18]1[CH:23]=[C:22]([CH2:24][C:25]2[CH:26]=[N:27][C:28](=[O:37])[N:29]([CH2:31][C:32]([OH:34])=[O:33])[CH:30]=2)[C:21](=[O:38])[N:20]=[C:19]1[S:39][CH2:40][C:41]1[CH:46]=[CH:45][C:44]([F:47])=[CH:43][CH:42]=1)=[O:16])[CH3:14])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 9896094HCID 9896094、化合物

生成物 1

HCID 9809899HCID 9809899、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 312751,4-Dioxane溶媒

実験手順

To a stirring solution of 1-(N-(1-dodecyl)-N-methylaminocarbonylmethyl)-2-(4-fluorobenzyl)thio-5-(1-ethoxycarbonylmethyl-2-oxopyrimid-5-ylmethyl)pyrimidin-4-one in 1,4-dioxan (8 ml) was added 0.5M sodium hydroxide (1.56 ml). After 1 h, water (3 ml) was added. After a further hour, the mixture was diluted with water, extracted with ethyl acetate and acidified to pH 3 with aq. sodium bisulphate. The solid which precipitated was filtered, washed with water and ether, heated briefly with acetone and filtered again to give the product as a white solid, yield 0.28 g. 1H-NMR (d6-DMSO) δ0.85 (3H, t), 1.22 (18H, m), 1.35-1.61 (2H, m,), 2.78, 2.95 (3H, 2xs), 3.20-3.35 (2H, m), 3.58 (2H, s), 4.40 (2H, s), 4.55 (2H, s), 4.83 (2H, m), 7.10 (2H, m), 7.44 (2H, m), 7.54 and 7.57 (1H, 2xs), 8.03 (1H, m), 8.54 (1H, m) 13.10 (1H, br. s); MS (APCI+) found (M+1)=642, C33H44FN5O5S requires 641.

後処理

  1. waitAfter a further hour
  2. extractionextracted with ethyl acetate
  3. customThe solid which precipitated
  4. filtrationwas filtered
  5. washwashed with water and ether
  6. temperatureheated briefly with acetone
  7. filtrationfiltered again

出典と根拠

ORDレコード
ord-500d92576f144b09aaf9814914bf06f9
出典データセット
uspto-grants-2003_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06559155B1

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート