Ammonia → 2-Butoxy-9-(3-bromopropyl)-7,8-dihydro-8-oxoadenine

HRID 1666199노트

반응식

HRID 1666199 반응식
[Br:1][CH2:2][CH2:3][CH2:4][N:5]1[C:13]([O:14]C)=[N:12][C:11]2[C:6]1=[N:7][C:8]([O:17][CH2:18][CH2:19][CH2:20][CH3:21])=[N:9][C:10]=2[NH2:16].Cl.N>CO.O1CCOCC1>[CH2:18]([O:17][C:8]1[N:7]=[C:6]2[C:11]([NH:12][C:13](=[O:14])[N:5]2[CH2:4][CH2:3][CH2:2][Br:1])=[C:10]([NH2:16])[N:9]=1)[CH2:19][CH2:20][CH3:21]

참가 물질

6

반응물 3

HCID 222AmmoniaHCID 313Hydrochloric AcidHCID 231584909-(3-Bromopropyl)-2-butoxy-8-methoxy-9H-purin-6-amine

생성물 1

HCID 592880312-Butoxy-9-(3-bromopropyl)-7,8-dihydro-8-oxoadenine수율 92%

시약·촉매·용매 2

HCID 887Methanol용매HCID 312751,4-Dioxane용매

실험 절차

To a solution of the compound (1 g, 2.79 mmol) obtained in Step (i) in methanol (2 ml) was added a 4N-hydrochloric acid in dioxane (2 ml), and the mixture was stirred at room temperature for 3.5 hours. The mixture was neutralized by addition of 28% aqueous ammonia at 0° C., and the mixture was stirred for one hour. The precipitated crystals were collected by filtration, washed twice with water (2 ml) and further washed twice with methanol (2 ml), and dried to give the subtitle compound (882 mg) as a white solid. Yield: 92%

후처리

  1. stirringthe mixture was stirred for one hour
  2. filtrationThe precipitated crystals were collected by filtration
  3. washwashed twice with water (2 ml)
  4. washfurther washed twice with methanol (2 ml)
  5. customdried

출처 및 근거

ORD 기록
ord-7481010a905a461d9e1c2415770efa28
출처 데이터셋
uspto-grants-2011_10
특허 번호
US08044056B2

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