Sodium Hydroxide → HCID 14257567, 화합물

HRID 2291952노트

반응식

HRID 2291952 반응식
[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]

참가 물질

7

반응물 4

HCID 14798Sodium HydroxideHCID 517165Ammonium AcetateHCID 5003444Sodium cyanoborohydrideHCID 14257566HCID 14257566, 화합물

생성물 1

HCID 14257567HCID 14257567, 화합물

시약·촉매·용매 2

HCID 887Methanol용매HCID 6212Chloroform용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-967116a071bc4e9d92a4bef28f294382
출처 데이터셋
uspto-grants-1989_01
특허 번호
US04798897

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