1,1'-(Chlorophenylmethylene)bis(4-methoxybenzene) → HCID 69621284, 화합물

HRID 547993노트

반응식

HRID 547993 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 69621284HCID 69621284, 화합물수율 80%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-3ed3f83621ea498b8afbb6fbb25f85e3
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07939677B2

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