1,4-Dioxa-8-azaspiro(4.5)decane → 8-(5-Chloropyrimidin-2-yl)-1,4-dioxa-8-azaspiro[4.5]decane

HRID 68790

反応式

HRID 68790 の反応式
[O:1]1[C:5]2([CH2:10][CH2:9][NH:8][CH2:7][CH2:6]2)[O:4][CH2:3][CH2:2]1.Cl[C:12]1[N:17]=[CH:16][C:15]([Cl:18])=[CH:14][N:13]=1>CN(C)C=O.O1CCOCC1.C(N(CC)CC)C>[Cl:18][C:15]1[CH:14]=[N:13][C:12]([N:8]2[CH2:9][CH2:10][C:5]3([O:4][CH2:3][CH2:2][O:1]3)[CH2:6][CH2:7]2)=[N:17][CH:16]=1

参加物

6

反応物 2

HCID 674351,4-Dioxa-8-azaspiro(4.5)decaneHCID 5906412,5-Dichloropyrimidine

生成物 1

HCID 682901798-(5-Chloropyrimidin-2-yl)-1,4-dioxa-8-azaspiro[4.5]decane

試薬・触媒・溶媒 3

HCID 6228Dimethylformamide溶媒HCID 8471Triethylamine溶媒HCID 312751,4-Dioxane溶媒

反応条件

温度
120 °C

実験手順

1,4-Dioxa-8-azaspiro[4.5]decane (2.39 g) is combined with 2,5-dichloropyrimidine (2.44 g) in N,N-dimethylformamide (50 mL), 1,4-dioxane (75 mL) and triethylamine (6.7 mL) in a glass pressure reaction vessel. The mixture is heated with stirring at 120° C. for 16 h. After cooling to room temperature, the solution is concentrated and partitioned between dichloromethane (100 mL) and water (100 mL). The aqueous layer is extracted with dichloromethane (100 mL). The dichloromethane layers are combined, washed with water (2×100 mL), dried over Na2SO4, filtered and concentrated to yield the title compound.

後処理

  1. temperatureThe mixture is heated
  2. temperatureAfter cooling to room temperature
  3. concentrationthe solution is concentrated
  4. custompartitioned between dichloromethane (100 mL) and water (100 mL)
  5. extractionThe aqueous layer is extracted with dichloromethane (100 mL)
  6. washwashed with water (2×100 mL)
  7. dry with materialdried over Na2SO4
  8. filtrationfiltered
  9. concentrationconcentrated

出典と根拠

ORDレコード
ord-9a58d179ff614bf0bd54c20ea26b7417
出典データセット
uspto-grants-2014_09
特許番号
US08822471B2

関連ノート

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