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Lithium Hydroxide → HCID 66924480, 화합물

HRID 1888169
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HRID 1888169 반응식
[N:1]1[N:2]=[N:3][N:4]2[CH:8]([C:9]([O:11]C)=[O:10])[CH2:7][CH2:6][C:5]=12.[Li+].[OH-]>C1COCC1.O.CO>[N:1]1[N:2]=[N:3][N:4]2[CH:8]([C:9]([OH:11])=[O:10])[CH2:7][CH2:6][C:5]=12
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참가 물질

4

반응물 2

HCID 3939Lithium HydroxideHCID 57907640HCID 57907640, 화합물

생성물 1

HCID 66924480HCID 66924480, 화합물

시약·촉매·용매 1

HCID 21892291Methanol tetrahydrofuran water용매

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온도
60 °C

실험 절차

To a solution of methyl 6,7-dihydro-5H-pyrrolo[1,2-d]tetrazole-5-carboxylate (300 mg, 1.78 mmol) from step B in THF/water/MeOH was added LiOH (214 mg, 8.92 mmol) and the resulting solution was heated via oil bath to 60° C. for 16 h. (Round bottom was equipped with a condenser.) The solution was cooled to room temperature and concentrated to remove organic solvents. The aqueous layer was then acidified to pH of ˜5 using 2.0 N aqueous HCl. The mixture was concentrated to dryness under vacuum, azeotroping with toluene (2×20 mL) to make sure all water was removed. The material was used without further purification with lithium chloride as a by-product. LC-MS: m/z (ES)=155 (MH)+.

후처리

  1. custom(Round bottom was equipped with a condenser.) The solution
  2. temperaturewas cooled to room temperature
  3. concentrationconcentrated
  4. customto remove organic solvents
  5. concentrationThe mixture was concentrated to dryness under vacuum
  6. customazeotroping with toluene (2×20 mL)
  7. customwas removed
  8. customThe material was used without further purification with lithium chloride as a by-product

출처 및 근거

ORD 기록
ord-0be298e00d9f410baf1bf242096c8248
출처 데이터셋
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08501786B2

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