1,1'-(Chlorophenylmethylene)bis(4-methoxybenzene) → HCID 69621284、化合物

HRID 254918ノート

反応式

HRID 254918 の反応式
[C@@H:1]1([N:10]2[CH:17]=[CH:16][C:14](=[O:15])[NH:13][C:11]2=[O:12])[S:7][C@H:6]([CH2:8][OH:9])[C@@H:4]([OH:5])[C@H:2]1[OH:3].[CH3:18][O:19][C:20]1[CH:41]=[CH:40][C:23]([C:24](Cl)([C:33]2[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=2)[C:25]2[CH:30]=[CH:29][C:28]([O:31][CH3:32])=[CH:27][CH:26]=2)=[CH:22][CH:21]=1>N1C=CC=CC=1>[CH3:32][O:31][C:28]1[CH:27]=[CH:26][C:25]([C:24]([CH:8]([OH:9])[C@H:6]2[S:7][C@@H:1]([N:10]3[CH:17]=[CH:16][C:14](=[O:15])[NH:13][C:11]3=[O:12])[C@H:2]([OH:3])[C@@H:4]2[OH:5])([C:33]2[CH:34]=[CH:35][CH:36]=[CH:37][CH:38]=2)[C:23]2[CH:40]=[CH:41][C:20]([O:19][CH3:18])=[CH:21][CH:22]=2)=[CH:30][CH:29]=1

参加物

4

反応物 2

HCID 968311,1'-(Chlorophenylmethylene)bis(4-methoxybenzene)HCID 112191494′-Thiouridine

生成物 1

HCID 69621284HCID 69621284、化合物収率 80%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

Compound 13 (2 g, 7.754 mmol) was dissolved in dry pyridine (20 mL), 4,4′-dimethoxytrityl chloride (2.9 g, 8.53 mmol) was added and the mixture stirred at room temperature overnight. The reaction was quenched with methanol and taken up in ethyl acetate (200 mL). The ethyl acetate solution was washed twice with saturated sodium bicarbonate solution, once with water, once with brine, and dried over anhydrous sodium sulfate. The solvents were removed under reduced pressure and the residue purified by flash chromatography (7% methanol in dichloromethane). The desired fractions were pooled and concentrated to give Compound 14 (3.0 g) in 80% yield. The structure of Compound 14 was confirmed by 1H NMR & ESMS.

後処理

  1. customThe reaction was quenched with methanol
  2. washThe ethyl acetate solution was washed twice with saturated sodium bicarbonate solution, once with water, once with brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. customThe solvents were removed under reduced pressure
  5. customthe residue purified by flash chromatography (7% methanol in dichloromethane)
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-8add7af64a9d425493d309b6ccb2492b
出典データセット
uspto-grants-2011_01
特許番号
US07875733B2

反応ノート

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