Water → Diphenylmethyl [3-fluoro-4,5-bis-[(2-methoxy-ethoxy)-methoxy]-phenyl]-hydroxy-acetate

HRID 727409

반응식

HRID 727409 반응식
[F:1][C:2]1[CH:3]=[C:4]([CH:22]([OH:26])[C:23]([OH:25])=[O:24])[CH:5]=[C:6]([O:15][CH2:16][O:17][CH2:18][CH2:19][O:20][CH3:21])[C:7]=1[O:8][CH2:9][O:10][CH2:11][CH2:12][O:13][CH3:14].[C:27]1([C:33]([C:36]2[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=2)=[N+]=[N-])[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1.O>ClCCl.CCOCC>[F:1][C:2]1[CH:3]=[C:4]([CH:22]([OH:26])[C:23]([O:25][CH:33]([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)[C:36]2[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=2)=[O:24])[CH:5]=[C:6]([O:15][CH2:16][O:17][CH2:18][CH2:19][O:20][CH3:21])[C:7]=1[O:8][CH2:9][O:10][CH2:11][CH2:12][O:13][CH3:14]

참가 물질

6

반응물 3

HCID 962WaterHCID 612301,1'-(Diazomethylene)bis(benzene)HCID 9951689[3-Fluoro-4,5-bis-[(2-methoxy-ethoxy)-methoxy]-phenyl]-hydroxy-acetic acid

생성물 1

HCID 9915375Diphenylmethyl [3-fluoro-4,5-bis-[(2-methoxy-ethoxy)-methoxy]-phenyl]-hydroxy-acetate

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 6344Dichloromethane용매

실험 절차

5.3 g of the acid of Step A were dissolved in 66 ml of dichloromethane and then 46 ml of a solution of diphenyl diazomethane at 6.5 g in ether were added at 15° C. The mixture was stirred for 16 hours at ambient temperature and then water was added, followed by decanting and acidifying with acetic acid. Washing with a saturated solution of sodium bicarbonate, drying and evaporating the solvents yielded after chromatography on silica and eluting with an ethyl acetate-hexane mixture (50-50) 4.0 g of the desired product with a Rf=0.17.

후처리

  1. customby decanting
  2. washWashing with a saturated solution of sodium bicarbonate
  3. customdrying
  4. customevaporating the solvents
  5. customyielded after chromatography on silica
  6. washeluting with an ethyl acetate-hexane mixture (50-50) 4.0 g of the desired product with a Rf=0.17

출처 및 근거

ORD 기록
ord-4e04f9953a1a4cf0ad91692008f20c87
출처 데이터셋
uspto-grants-1998_01
특허 번호
US05712266

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