Diisopropylethylamine → HCID 70981090, 화합물

HRID 2280749노트

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HRID 2280749 반응식
[C:1]([NH:5][C:6]1[C:11]([C:12](O)=[O:13])=[CH:10][N:9]=[C:8]([S:15][CH3:16])[N:7]=1)([CH3:4])([CH3:3])[CH3:2].C[N:18](C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.Cl.N.CCN(C(C)C)C(C)C>CN(C=O)C>[C:1]([NH:5][C:6]1[C:11]([C:12]([NH2:18])=[O:13])=[CH:10][N:9]=[C:8]([S:15][CH3:16])[N:7]=1)([CH3:4])([CH3:3])[CH3:2]

참가 물질

6

반응물 4

HCID 81531DiisopropylethylamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 12820921Azane;hydrochlorideHCID 70981544HCID 70981544, 화합물

생성물 1

HCID 70981090HCID 70981090, 화합물수율 90.1%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

4-(tert-Butylamino)-2-(methylthio)pyrimidine-5-carboxylic acid (2.83 g, 11.73 mmol) and 2-(3H-[1,2,3]triazolo[4,5-b]pyridin-3-yl)-1,1,3,3-tetramethylisouronium hexafluoro-phosphate(V) (6.69 g, 17.59 mmol) were combined in a 250 mL round-bottomed flask followed by the addition of DMF (29 mL). After that ammonia hydrochloride-(3.14 g, 58.6 mmol) and DIEA (10.21 mL, 58.6 mmol) were added and the mixture was stirred at room temperature overnight. The solvent was concentrated under reduced pressure and water (150 mL) was added. The resulting suspension was filtered, washed with water and dried under high vacuum overnight to afford 4-(tert-butylamino)-2-(methylthio)-pyrimidine-5-carboxamide (2.54 g, 10.57 mmol, 90% yield). MS (ESI) m/z 241.2

후처리

  1. concentrationThe solvent was concentrated under reduced pressure and water (150 mL)
  2. additionwas added
  3. filtrationThe resulting suspension was filtered
  4. washwashed with water
  5. customdried under high vacuum overnight

출처 및 근거

ORD 기록
ord-b11d49de2b7b4836980c65505ecf2aee
출처 데이터셋
uspto-grants-2015_09
특허 번호
US09139534B2

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