Water → 8,8'-(2,5-Dichloropyrimidine-4,6-diyl)bis(3-oxa-8-azabicyclo[3.2.1]octane)

HRID 75452

反応式

HRID 75452 の反応式
[Cl:1][C:2]1[N:7]=[C:6](Cl)[C:5]([Cl:9])=[C:4](Cl)[N:3]=1.[CH:11]12[NH:18][CH:15]([CH2:16][CH2:17]1)[CH2:14][O:13][CH2:12]2.[OH2:19]>C1COCC1.C(N(CC)CC)C>[Cl:1][C:2]1[N:7]=[C:6]([N:18]2[CH:15]3[CH2:16][CH2:17][CH:11]2[CH2:12][O:13][CH2:14]3)[C:5]([Cl:9])=[C:4]([N:18]2[CH:11]3[CH2:17][CH2:16][CH:15]2[CH2:14][O:19][CH2:12]3)[N:3]=1

参加物

6

反応物 3

HCID 962Water2 回HCID 156902,4,5,6-TetrachloropyrimidineHCID 152351793-Oxa-8-azabicyclo(3.2.1)octane

生成物 1

HCID 866659028,8'-(2,5-Dichloropyrimidine-4,6-diyl)bis(3-oxa-8-azabicyclo[3.2.1]octane)

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 8471Triethylamine溶媒

実験手順

To a solution of 2,4,5,6-tetrachloro-pyrimidine (2.0 g, 9.2 mmol) in THF (20 mL) and triethylamine (excess) was added 3-oxa-8-aza-bicyclo[3.2.1]octane (2.7 g, 18 mmol) at −78° C. The reaction slowly warmed to room temperature and a white precipitate formed. To the reaction was added water (2.0 mL) and the mixture was refluxed for three days. The reaction was cooled and water was added to precipitate a white solid. The solids were collected by filtration and washed with diethyl ether to yield the title compound (2.0 g). MS m/z=372 (M+H).

後処理

  1. customThe reaction
  2. customa white precipitate formed
  3. temperaturethe mixture was refluxed for three days
  4. temperatureThe reaction was cooled
  5. customto precipitate a white solid
  6. filtrationThe solids were collected by filtration
  7. washwashed with diethyl ether

出典と根拠

ORDレコード
ord-451997b8ecc143308e17e807e39f5ea7
出典データセット
uspto-grants-2014_09
特許番号
US08835429B2

関連ノート

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