Water → 2-(2-chloro-7H-pyrrolo[2,3-d]pyrimidin-7-yl)-1-morpholinoethanone

HRID 1051522노트

반응식

HRID 1051522 반응식
[Cl:1][C:2]1[N:3]=[CH:4][C:5]2[CH:10]=[CH:9][N:8]([CH2:11][C:12]([OH:14])=O)[C:6]=2[N:7]=1.CN(C(ON1N=N[C:25]2C=[CH:27][CH:28]=[N:29][C:24]1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.[OH2:39]>C(Cl)Cl>[Cl:1][C:2]1[N:3]=[CH:4][C:5]2[CH:10]=[CH:9][N:8]([CH2:11][C:12]([N:29]3[CH2:24][CH2:25][O:39][CH2:27][CH2:28]3)=[O:14])[C:6]=2[N:7]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 867292892-(2-chloro-7H-pyrrolo[2,3-d]pyrimidin-7-yl)acetic acid

생성물 1

HCID 867292902-(2-chloro-7H-pyrrolo[2,3-d]pyrimidin-7-yl)-1-morpholinoethanone수율 80%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of 2-(2-chloro-7H-pyrrolo[2,3-d]pyrimidin-7-yl)acetic acid (100 mg, 0.474 mmol), amine (15.4 mg, 0.496 mmol), HATU (79 mg, 0.59 mmol) and TEA (95.8 mg, 0.0.948 mmol) in DCM (10 mL) was stirred at room temperature for 2 h. Upon completion of the reaction, water was added to the mixture and extracted with DCM. The organic layer was dried over anhydrous Na2SO4, filtered and concentrated, producing a the desired product which used directly in the next step without further purification (100 mg, Yield 80%). LCMS (m/z): 281.1 (M+1).

후처리

  1. additionwas added to the mixture
  2. extractionextracted with DCM
  3. dry with materialThe organic layer was dried over anhydrous Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-77fefb17a157471e9ff21ab9e99658fd
출처 데이터셋
uspto-grants-2016_07
특허 번호
US09388173B2

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