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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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HCID 15292629, 화합물 → HCID 131719743, 화합물

HRID 1080632
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HRID 1080632 반응식
Cl.[NH2:2][CH2:3][CH2:4][O:5][NH2:6].[OH:7][C@H:8]1[CH2:25][CH2:24][C@@:23]2([CH3:26])[C@H:10]([CH2:11][CH2:12][C@@H:13]3[C@@H:22]2[CH2:21][CH2:20][C@@:18]2([CH3:19])[C@:14]3([OH:30])[CH2:15][CH2:16][C@@H:17]2[CH2:27][CH:28]=O)[CH2:9]1>[OH-].[Na+].O1CCOCC1>[NH2:2][CH2:3][CH2:4][O:5][N:6]=[CH:28][CH2:27][C@H:17]1[CH2:16][CH2:15][C@:14]2([OH:30])[C@H:13]3[C@H:22]([CH2:21][CH2:20][C@:18]12[CH3:19])[C@:23]1([CH3:26])[C@@H:10]([CH2:9][C@@H:8]([OH:7])[CH2:25][CH2:24]1)[CH2:11][CH2:12]3
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참가 물질

5

반응물 2

HCID 15292629HCID 15292629, 화합물HCID 233652242-(Aminooxy)ethanamine hydrochloride

생성물 1

HCID 131719743HCID 131719743, 화합물수율 52.7%

시약·촉매·용매 2

HCID 14798Sodium Hydroxide용매HCID 312751,4-Dioxane용매2회

실험 절차

To a solution of 0.47 g of 2-aminoethoxyamine hydrochloride in 16 ml of 1N NaOH and 20 ml of dioxane a solution of 0.89 g of 3β,14β-dihydroxy-5β-androstane-17β-ylacetaldehyde (Prepn. 2) in 15 ml of dioxane was added at room temperature. After 20 hrs the solution was extracted with ethyl acetate; the organic layer was dried over anhydrous sodium sulfate and evaporated to dryness. The crude product was purified by flash chromatography (SiO2) using chloroform with increasing amounts of methanol (6 to 20%) as the eluant. The fractions containing the title compound were collected and evaporated to dryness. The residue was ground with di-iso-propyl ether to give 0.55 g of the title compound (I-bf), as a white foam.

후처리

  1. extractionAfter 20 hrs the solution was extracted with ethyl acetate
  2. dry with materialthe organic layer was dried over anhydrous sodium sulfate
  3. customevaporated to dryness
  4. customThe crude product was purified by flash chromatography (SiO2)
  5. additionThe fractions containing the title compound
  6. customwere collected
  7. customevaporated to dryness

출처 및 근거

ORD 기록
ord-e3561d84c3754cf0943c1167493f7d35
출처 데이터셋
uspto-grants-1996_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05583127

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