Sodium Hydroxide → HCID 14257567、化合物

HRID 2291952ノート

反応式

HRID 2291952 の反応式
[CH2:1]([N:5]([CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH3:24])[S:6]([C:9]1[C:10]2[CH:11]=[CH:12][N:13]=[CH:14][C:15]=2[CH:16]=[CH:17][CH:18]=1)(=[O:8])=[O:7])[C:2]([CH3:4])=O.C([O-])(=O)C.[NH4+].C([BH3-])#[N:31].[Na+].[OH-].[Na+]>C(Cl)(Cl)Cl.CO>[NH2:31][CH:2]([CH3:4])[CH2:1][N:5]([CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH3:24])[S:6]([C:9]1[C:10]2[CH:11]=[CH:12][N:13]=[CH:14][C:15]=2[CH:16]=[CH:17][CH:18]=1)(=[O:8])=[O:7]

参加物

7

反応物 4

HCID 14798Sodium HydroxideHCID 517165Ammonium AcetateHCID 5003444Sodium cyanoborohydrideHCID 14257566HCID 14257566、化合物

生成物 1

HCID 14257567HCID 14257567、化合物

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6212Chloroform溶媒

実験手順

To 75 ml of an anhydrous methanol solution containing 5.89 g of the thus obtained N-acetonyl-N-hexyl-5-isoquinolinesulfonamide were added 13.03 g of ammonium acetate and 0.75 g of sodium cyanoborohydride, followed by stirring at 15° to 20° C. for 19 hours. Then, the methanol was removed at 30° C. under reduced pressure. To the resultant reaction product were added 50 ml of chloroform and 50 ml of 1N sodium hydroxide solution. The chloroform layer was dried with anhydrous magnesium sulfate, and the chloroform was removed under reduced pressure to obtain a residue. The residue thus obtained was subjected to purification by silica gel column chromatography (Wacogel C-200, 100 g; solvent: chloroform) to obtain 2.75 g of N-(2-aminopropyl)-N-hexyl-5-isoquinolinesulfonamide [Compound (11)]. Compound (11) was analyzed to give the following data.

後処理

  1. customThen, the methanol was removed at 30° C. under reduced pressure
  2. customTo the resultant reaction product
  3. dry with materialThe chloroform layer was dried with anhydrous magnesium sulfate
  4. customthe chloroform was removed under reduced pressure
  5. customto obtain a residue
  6. customThe residue thus obtained
  7. customwas subjected to purification by silica gel column chromatography (Wacogel C-200, 100 g; solvent: chloroform)

出典と根拠

ORDレコード
ord-967116a071bc4e9d92a4bef28f294382
出典データセット
uspto-grants-1989_01
特許番号
US04798897

反応ノート

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