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Hydrochloric Acid → HCID 86590609、化合物

HRID 1725583
ノート
印刷プレビュー

反応式

HRID 1725583 の反応式
C[O:2][C:3]1C=C(C=C[C:10]=1OCC1C=CC(OC)=CC=1)C=O.C[O-].[Na+].Cl.[NH:25]([CH:32]=[C:33]([CH2:36][C:37]1[CH:42]=[CH:41][C:40]([O:43][CH2:44][C:45]2[CH:50]=[CH:49][C:48]([O:51][CH3:52])=[CH:47][CH:46]=2)=[C:39]([O:53][CH3:54])[CH:38]=1)[C:34]#[N:35])[C:26]1C=CC=C[CH:27]=1>CS(C)=O.ClCCl.O>[CH3:54][O:53][C:39]1[CH:38]=[C:37]([CH:42]=[CH:41][C:40]=1[O:43][CH2:44][C:45]1[CH:46]=[CH:47][C:48]([O:51][CH3:52])=[CH:49][CH:50]=1)[CH2:36][C:33](=[CH:32][N:25]1[CH2:26][CH2:27][O:2][CH2:3][CH2:10]1)[C:34]#[N:35]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 27644923-Methoxy-4-[(4-methoxyphenyl)methoxy]benzaldehydeHCID 10942334Sodium MethoxideHCID 69006529HCID 69006529、化合物

生成物 1

HCID 86590609HCID 86590609、化合物

試薬・触媒・溶媒 3

HCID 679Dimethyl Sulfoxide溶媒
HCID 962
Water
溶媒
HCID 6344Dichloromethane溶媒

実験手順

3-Methoxy-4-[(4-methoxybenzyl)oxy]benzaldehyde (20.0 g, 73.4 mmol) and 3-morpholinopropronitrile (Lancaster, 11.0 g, 77.1 mmol) were stirred in DMSO (15 mL) at 65 C until the mixture was homogeneous. The solution was cooled to 40 C and sodium methoxide (0.79 g, 14.7 mmol) was added. The mixture was stirred at 75 C for 15 minutes, then cooled to room temperature and diluted with dichloromethane (150 mL) and water (200 mL). 1N HCl (25 mL) was added and the two layers were seperated. The organics were combined and dried (magnesium sulfate), filtered and concentrated to a red oil (29.5 g, 73 mmol) that was used directly in the synthesis of 3-anilino-2-{3-methoxy-4-[(4-methoxybenzyl)oxy]benzyl}prop-2-enenitrile. 1H NMR (300 MHz, d6-DMSO): δ 7.38 (d, 2H), 7.03-6.95 (m,3H), 6.84 (t, J=13.5 Hz, 2H), 6.73 (d, J=8.2 Hz, 1H), 4.98 (s, 3H), 3.78 (s, 3H), 3.76 (s, 3H), 3.66-3.60 (m, 2H), 3.55-3.50 (m, 3H), 3.46-3.43 (m, 2H), 3.36 (s, 1H), 3.33-3.29 (m, 2H). MS (ES+, m/z)=395 (M+H).

後処理

  1. additionwas added
  2. customthe two layers were seperated
  3. dry with materialdried (magnesium sulfate)
  4. filtrationfiltered

出典と根拠

ORDレコード
ord-cff3f35122464fdb8079e68c06cecdaa
出典データセット
uspto-grants-2009_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07491731B2

反応ノート

読み込み中…

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