Sodium Hydroxide → HCID 178450080, 화합물

HRID 1368554노트

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HRID 1368554 반응식
C1(C(=[N:14][C:15]2[CH:16]=[C:17]3[C:22](=[CH:23][CH:24]=2)[CH:21]=[C:20]([C:25]([C:30]2[N:31]=[CH:32][N:33](C(C4C=CC=CC=4)(C4C=CC=CC=4)C4C=CC=CC=4)[CH:34]=2)([OH:29])[CH:26]([CH3:28])[CH3:27])[CH:19]=[CH:18]3)C2C=CC=CC=2)C=CC=CC=1.NC1C=C2C(=CC=1)C=C(C(C1N=CN(C(C3C=CC=CC=3)(C3C=CC=CC=3)C3C=CC=CC=3)C=1)(O)C(C)C)C=C2.[CH3:94][S:95](Cl)(=[O:97])=[O:96].[OH-].[Na+]>ClCCl.N1C=CC=CC=1>[OH:29][C:25]([C:20]1[CH:21]=[C:22]2[C:17](=[CH:18][CH:19]=1)[CH:16]=[C:15]([NH:14][S:95]([CH3:94])(=[O:97])=[O:96])[CH:24]=[CH:23]2)([C:30]1[N:31]=[CH:32][NH:33][CH:34]=1)[CH:26]([CH3:28])[CH3:27]

참가 물질

7

반응물 4

HCID 14798Sodium HydroxideHCID 31297Methanesulfonyl chlorideHCID 22018326HCID 22018326, 화합물HCID 22018411HCID 22018411, 화합물

생성물 1

HCID 178450080HCID 178450080, 화합물

시약·촉매·용매 2

HCID 1049Pyridine용매HCID 6344Dichloromethane용매

실험 절차

In a similar manner to that described in Example 51-(ii), a reaction was carried out by using 1-{6-[(diphenylmethylene)amino]naphthalen-2-yl}-2-methyl-1-(1-trityl-1H-imidazol-4-yl)-1-propanol (2.0 g) to give crude product containing 1-(6-aminonaphthalen-2-yl)-2-methyl-1-(1-trityl-1H-imidazol-4-yl)-1-propanol as a pale yellow oily substance. The crude product was dissolved in dichloromethane (10 ml). To the solution were added pyridine (0.71 ml) and methanesulfonyl chloride (0.34 ml) under ice cooling, and the mixture was stirred for 30 min. To the mixture was added 0.1N-aqueous solution of sodium hydroxide, and the mixture was extracted with ethyl acetate, washed with saturated sodium chloride solution and dried. The solvent was distilled off. The residue was purified by column chromatography (eluent, hexane:ethyl acetate=1:1) to give the titled compound (1.16 g) as a pale yellow powder.

후처리

  1. customto give crude product
  2. extractionthe mixture was extracted with ethyl acetate
  3. washwashed with saturated sodium chloride solution
  4. customdried
  5. distillationThe solvent was distilled off
  6. customThe residue was purified by column chromatography (eluent, hexane:ethyl acetate=1:1)

출처 및 근거

ORD 기록
ord-fef7cdf58c1d49308e8f0e18adb93ee2
출처 데이터셋
uspto-grants-2003_06
특허 번호
US06573289B1

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