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Lithium hydroxide, monohydrate → HCID 86713331, 화합물

HRID 928002
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HRID 928002 반응식
[NH2:1][C:2]1[C:11]([C:12]([O:14]C)=[O:13])=[C:10]2[C:5]([CH:6]3[CH2:16][CH:7]3[CH2:8][O:9]2)=[CH:4][CH:3]=1.O.[OH-].[Li+]>O1CCOCC1.O>[NH2:1][C:2]1[C:11]([C:12]([OH:14])=[O:13])=[C:10]2[C:5]([CH:6]3[CH2:16][CH:7]3[CH2:8][O:9]2)=[CH:4][CH:3]=1
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참가 물질

5

반응물 2

HCID 168937Lithium hydroxide, monohydrateHCID 86713293Methyl 5-amino-1,1a,2,7b-tetrahydrocyclopropa[c]chromene-4-carboxylate2회

생성물 1

HCID 86713331HCID 86713331, 화합물수율 103.6%

시약·촉매·용매 2

HCID 962Water용매HCID 312751,4-Dioxane용매

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온도
90 °C

실험 절차

A mixture of methyl (1aRS,7bSR)-5-amino-1,1a,2,7b-tetrahydrocyclopropa[c]chromene-4-carboxylate (Intermediate 42, 1.0 g) and lithium hydroxide monohydrate (0.96 g) in dioxane (16 mL) and water (14 mL) was stirred and heated at 90° C. for 1 hour. After cooling, the mixture was concentrated under vacuum and the residue was diluted with water and neutralised to pH7 with formic acid. The mixture was then extracted with ethyl acetate, dried (Na2SO4) and filtered and the filtrate was evaporated to dryness to give (1aRS,7bSR)-5-amino-1,1a,2,7b-tetrahydro-cyclopropa-[c]chromene-4-carboxylic acid (0.97 g) as a yellow oil.

후처리

  1. temperatureAfter cooling
  2. concentrationthe mixture was concentrated under vacuum
  3. additionthe residue was diluted with water and neutralised to pH7 with formic acid
  4. extractionThe mixture was then extracted with ethyl acetate
  5. dry with materialdried (Na2SO4)
  6. filtrationfiltered
  7. customthe filtrate was evaporated to dryness

출처 및 근거

ORD 기록
ord-ff7d7f0c85dd4b46aafd76b4ce16d5d4
출처 데이터셋
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09290472B2

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