N-(4-Bromobutyl)phthalimide → 4-Amino-2-(4-phthalimidobutylthio)pyrimidine

HRID 34778

反応式

HRID 34778 の反応式
[NH:1]1[CH:8]=[CH:7][C:5]([NH2:6])=[N:4][C:2]1=[S:3].N12CCCCC1C=NCCC2.Br[CH2:21][CH2:22][CH2:23][CH2:24][N:25]1[C:29](=[O:30])[C:28]2=[CH:31][CH:32]=[CH:33][CH:34]=[C:27]2[C:26]1=[O:35]>C(O)C>[NH2:6][C:5]1[CH:7]=[CH:8][N:1]=[C:2]([S:3][CH2:21][CH2:22][CH2:23][CH2:24][N:25]2[C:29](=[O:30])[C:28]3=[CH:31][CH:32]=[CH:33][CH:34]=[C:27]3[C:26]2=[O:35])[N:4]=1

参加物

5

反応物 3

HCID 93575N-(4-Bromobutyl)phthalimideHCID 3141121,5-Diazabicyclo(5,4,0)undec-5-eneHCID 178507915HCID 178507915、化合物

生成物 1

HCID 212987544-Amino-2-(4-phthalimidobutylthio)pyrimidine収率 86.7%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 2-thiocytosine (0.25 g.), 1,5-diazabicyclo[5,4,0]undec-5-ene (0.33 g.), ethanol (10 ml.) and N-(4-bromobutyl)phthalimide (0.62 g.) was stirred at room temperature for 18 hours and then evaporated to dryness. The residue was partitioned between water and ethyl acetate and the ethyl acetate phase was dried and evaporated to dryness. The residue was recrystallised from acetonitrile to give 4-amino-2-(4-phthalimidobutylthio)pyrimidine (0.56 g.), m.p. 164°-167°.

後処理

  1. customevaporated to dryness
  2. customThe residue was partitioned between water and ethyl acetate
  3. dry with materialthe ethyl acetate phase was dried
  4. customevaporated to dryness
  5. customThe residue was recrystallised from acetonitrile

出典と根拠

ORDレコード
ord-a682a20e344347838a09dbb729f50832
出典データセット
uspto-grants-1988_08
特許番号
US04762932

関連ノート

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