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Sodium Hydroxide → HCID 21913806、化合物

HRID 1008082
ノート
印刷プレビュー

反応式

HRID 1008082 の反応式
C([O:3][C:4](=[O:34])[C:5]1[CH:10]=[CH:9][C:8]([S:11]([CH2:14][CH2:15][CH2:16][N:17]2[C:25]3[C:24]([CH3:26])=[C:23]([CH3:27])[N:22]4[N:28]=[N:29][N:30]=[C:21]4[C:20]=3[N:19]=[C:18]2[CH2:31][CH2:32][CH3:33])(=[O:13])=[O:12])=[CH:7][CH:6]=1)C.[OH-].[Na+]>C(O)C>[CH3:27][C:23]1[N:22]2[N:28]=[N:29][N:30]=[C:21]2[C:20]2[N:19]=[C:18]([CH2:31][CH2:32][CH3:33])[N:17]([CH2:16][CH2:15][CH2:14][S:11]([C:8]3[CH:9]=[CH:10][C:5]([C:4]([OH:34])=[O:3])=[CH:6][CH:7]=3)(=[O:12])=[O:13])[C:25]=2[C:24]=1[CH3:26]
参加物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 14798Sodium HydroxideHCID 69412152HCID 69412152、化合物

生成物 1

HCID 21913806HCID 21913806、化合物収率 95.9%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

4-[3-(5,6-Dimethyl-8-propyl-7H-imidazo[4,5-c]tetrazolo[1,5-a]pyridin-7-yl)propane-1-sulfonyl]benzoic acid ethyl ester (2.50 g, 5.16 mmol), prepared as described in Parts A-E of Example 92 using the modification of Example 99, was treated with aqueous sodium hydroxide (10 mL of 1 N) in ethanol (26 mL), and the reaction stirred for two hours and became homogeneous. The solvents were removed under reduced pressure, and the residual white solid was dissolved in water (50 mL). The solution was washed with ethyl acetate (3×10 mL) and then adjusted to pH 4 with the addition of concentrated hydrochloric acid. A white solid precipitated, which was isolated by filtration, washed with water, and dried for three hours in a vacuum oven at 60° C. to provide 2.26 g of 4-[3-(5,6-dimethyl-8-propyl-7H-imidazo[4,5-c]tetrazolo[1,5-a]pyridin-7-yl)propane-1-sulfonyl]benzoic acid as a white solid.

後処理

  1. customThe solvents were removed under reduced pressure
  2. dissolutionthe residual white solid was dissolved in water (50 mL)
  3. washThe solution was washed with ethyl acetate (3×10 mL)
  4. additionadjusted to pH 4 with the addition of concentrated hydrochloric acid
  5. customA white solid precipitated
  6. customwhich was isolated by filtration
  7. washwashed with water
  8. customdried for three hours in a vacuum oven at 60° C.

出典と根拠

ORDレコード
ord-5c244df5288249ac9ee011aeeef81eab
出典データセット
uspto-grants-2004_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06797718B2

反応ノート

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