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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Hydrochloric Acid → 1-[(E)-[(E)-3-[(3S,5R,8R,9S,10S,13R,14S,17R)-3,14-dihydroxy-10,13-dimethyl-1,2,3,4,5,6,7,8,9,11,12,15,16,17-tetradecahydrocyclopenta[a]phenanthren-17-yl]-2-methylprop-2-enylidene]amino]guanidine

HRID 725259
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인쇄 미리보기

반응식

HRID 725259 반응식
C(=O)(O)O.[NH2:5][NH:6][C:7]([NH2:9])=[NH:8].Cl.[OH:11][C@H:12]1[CH2:33][CH2:32][C@@:31]2([CH3:34])[C@H:14]([CH2:15][CH2:16][C@@H:17]3[C@@H:30]2[CH2:29][CH2:28][C@@:27]2([CH3:35])[C@:18]3([OH:36])[CH2:19][CH2:20][C@@H:21]2/[CH:22]=[C:23](\[CH3:26])/[CH:24]=O)[CH2:13]1>O.O1CCOCC1>[NH:6](/[N:5]=[CH:24]/[C:23](/[CH3:26])=[CH:22]/[C@H:21]1[CH2:20][CH2:19][C@:18]2([OH:36])[C@H:17]3[C@H:30]([CH2:29][CH2:28][C@:27]12[CH3:35])[C@:31]1([CH3:34])[C@@H:14]([CH2:13][C@@H:12]([OH:11])[CH2:33][CH2:32]1)[CH2:15][CH2:16]3)[C:7]([NH2:9])=[NH:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 10666253(E)-3beta,14beta-dihydroxy-21-methyl-5beta-pregn-20-ene-21-carboxaldehydeHCID 178513185HCID 178513185, 화합물

생성물 1

HCID 1765375471-[(E)-[(E)-3-[(3S,5R,8R,9S,10S,13R,14S,17R)-3,14-dihydroxy-10,13-dimethyl-1,2,3,4,5,6,7,8,9,11,12,15,16,17-tetradecahydrocyclopenta[a]phenanthren-17-yl]-2-methylprop-2-enylidene]amino]guanidine수율 68.3%

시약·촉매·용매 2

HCID 962Water용매
HCID 312751,4-Dioxane용매2회

실험 절차

A mixture of 0.50 g of aminoguanidine hydrogencarbonate in 10 ml of water and 30 ml of dioxane was made acid to pH 3 with 3N HCl. A solution of 0.95 g of (E)-3β,14β-dihydroxy-21-methyl-5β-pregn-20-ene-21-carboxaldehyde (Prepn. 1) in 10 ml of dioxane was added at room temperature. After 3 days the mixture was evaporated to dryness under reduced pressure. The crude product was purified by flash chromatography (SiO2) using chloroform/methanol/28% ammonium hydroxide 80/20/3 as the eluant: the fractions containing the title compound were collected and evaporated to dryness. The residue was ground with diethyl ether and ethanol to give 0.75 g of the title compound (I-aa) as a white solid.

후처리

  1. customAfter 3 days the mixture was evaporated to dryness under reduced pressure
  2. customThe crude product was purified by flash chromatography (SiO2)
  3. additionthe fractions containing the title compound
  4. customwere collected
  5. customevaporated to dryness

출처 및 근거

ORD 기록
ord-6280d3e33d7e42d29f4bb246ba4d1112
출처 데이터셋
uspto-grants-1998_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05705662

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