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Lithium Hydroxide → HCID 66924480、化合物

HRID 1947701
ノート
印刷プレビュー

反応式

HRID 1947701 の反応式
[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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 3939Lithium HydroxideHCID 57907640HCID 57907640、化合物

生成物 1

HCID 66924480HCID 66924480、化合物

試薬・触媒・溶媒 1

HCID 21892291Methanol tetrahydrofuran water溶媒

反応条件

温度
60 °C

実験手順

To a solution of methyl 6,7-dihydro-5H-pyrrolo[1,2-d]tetrazole-5-carboxylate (300 mg, 1.78 mmol) 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 2N 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)+.

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート

後処理

  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

出典と根拠

ORDレコード
ord-7a6d1868dcd34b75b542facf4b523dd3
出典データセット
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08399480B2

反応ノート

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