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

HRID 68790

반응식

HRID 68790 반응식
[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

참가 물질

6

반응물 2

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

생성물 1

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

시약·촉매·용매 3

HCID 6228Dimethylformamide용매HCID 8471Triethylamine용매HCID 312751,4-Dioxane용매

반응 조건

온도
120 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9a58d179ff614bf0bd54c20ea26b7417
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822471B2

연결된 노트

불러오는 중…