Hydrochloric Acid → 6-Amino-2-butylamino-9-(tetrahydro-2H-Pyran-4-ylmethyl)-7,9-dihydro-8H-Purin-8-one

HRID 1011150

반응식

HRID 1011150 반응식
[CH2:1]([NH:5][C:6]1[N:14]=[C:13]2[C:9]([N:10]=[C:11]([O:22]C)[N:12]2[CH2:15][CH:16]2[CH2:21][CH2:20][O:19][CH2:18][CH2:17]2)=[C:8]([NH2:24])[N:7]=1)[CH2:2][CH2:3][CH3:4].Cl.[OH-].[Na+]>CO.O1CCOCC1>[NH2:24][C:8]1[N:7]=[C:6]([NH:5][CH2:1][CH2:2][CH2:3][CH3:4])[N:14]=[C:13]2[C:9]=1[NH:10][C:11](=[O:22])[N:12]2[CH2:15][CH:16]1[CH2:17][CH2:18][O:19][CH2:20][CH2:21]1

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 57699729N2-Butyl-8-methoxy-9-(tetrahydro-2H-pyran-4-ylmethyl)-9H-Purine-2,6-diamine

생성물 1

HCID 248845276-Amino-2-butylamino-9-(tetrahydro-2H-Pyran-4-ylmethyl)-7,9-dihydro-8H-Purin-8-one수율 57.2%

시약·촉매·용매 2

HCID 887Methanol용매HCID 312751,4-Dioxane용매

실험 절차

To a solution of N2-butyl-8-methoxy-9-(tetrahydro-2H-pyran-4-ylmethyl)-9H-purine-2,6-diamine (310 mg) in dry methanol (30 ml) at room temperature and under nitrogen was added 4.0M hydrogen chloride in 1,4-dioxane (5.5 ml) in one go. The reaction was left to stir at room temperature for 16 hours. The reaction was neutralised by the addition of 2.0M sodium hydroxide solution and concentrated in vacuo. The residue was taken up in water (10 ml) and the solid filtered and dried on the rotary evaporator (60° C.) for 30 minutes. This afforded the title compound as a solid (170 mg).

후처리

  1. waitThe reaction was left
  2. concentrationconcentrated in vacuo
  3. filtrationthe solid filtered
  4. customdried on the rotary evaporator (60° C.) for 30 minutes

출처 및 근거

ORD 기록
ord-607006ab63754d7796a344b7aac7b5ba
출처 데이터셋
uspto-grants-2011_07
특허 번호
US07977344B2

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