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Hydrochloric Acid → RS-93522

HRID 2074033
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HRID 2074033 반응식
[CH3:1][C:2]1[NH:3][C:4]([CH3:41])=[C:5]([C:21]([O:23][CH2:24][CH2:25][C:26]2[CH:31]=[CH:30][C:29]([O:32][CH2:33][CH:34]3[CH2:38][O:37]C(C)(C)[O:35]3)=[CH:28][CH:27]=2)=[O:22])[CH:6]([C:12]2[CH:17]=[CH:16][CH:15]=[C:14]([N+:18]([O-:20])=[O:19])[CH:13]=2)[C:7]=1[C:8]([O:10][CH3:11])=[O:9].Cl>CC(C)=O.O>[CH3:1][C:2]1[NH:3][C:4]([CH3:41])=[C:5]([C:21]([O:23][CH2:24][CH2:25][C:26]2[CH:31]=[CH:30][C:29]([O:32][CH2:33][CH:34]([OH:35])[CH2:38][OH:37])=[CH:28][CH:27]=2)=[O:22])[CH:6]([C:12]2[CH:17]=[CH:16][CH:15]=[C:14]([N+:18]([O-:20])=[O:19])[CH:13]=2)[C:7]=1[C:8]([O:10][CH3:11])=[O:9]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 136325642,6-Dimethyl-3-methoxycarbonyl-4-(3-nitrophenyl)-5-(2-[4-(2,2-dimethyl-1,3-dioxolan-4-yl)methoxyphenyl]ethoxycarbonyl)-1,4-dihydropyridine

생성물 1

HCID 128487RS-93522

시약·촉매·용매 2

HCID 180Acetone용매HCID 962Water용매2회

실험 절차

A solution of 21 g of 2,6-dimethyl-3-methoxycarbonyl-4-(3-nitrophenyl)-5-(2-[4-(2,2-dimethyl-1,3-dioxolan-4-yl)methoxyphenyl]ethoxycarbonyl)-1,4-dihydropyridine in 150 mL of acetone and 50 mL of water is treated with 10 mL of hydrochloric acid and the mixture heated at reflux for 6 h. Water (500 mL) is added and the mixture was extracted with ether. The ether layer is dried over Na2SO4 and evaporated to an oil which is purified by medium pressure chromatography on silica gel (90% ethyl acetate-hexane) to give 2,6-dimethyl-3-methoxycarbonyl-4-(3-nitrophenyl)-5-(2-[4-(2,3-dihydroxypropoxy)phenyl]ethoxycarbonyl)-1,4-dihydropyridine, m.p. 117-118° C., [α]D =-33.5°.

후처리

  1. temperaturethe mixture heated
  2. temperatureat reflux for 6 h
  3. extractionthe mixture was extracted with ether
  4. dry with materialThe ether layer is dried over Na2SO4
  5. customevaporated to an oil which
  6. customis purified by medium pressure chromatography on silica gel (90% ethyl acetate-hexane)

출처 및 근거

ORD 기록
ord-7c911318d64e4639acc0b07ef552f76f
출처 데이터셋
uspto-grants-1990_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04920225

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