Diisopropylethylamine → HCID 70981090、化合物

HRID 2280749ノート

反応式

HRID 2280749 の反応式
[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]

参加物

6

反応物 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、化合物

生成物 1

HCID 70981090HCID 70981090、化合物収率 90.1%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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

後処理

  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

出典と根拠

ORDレコード
ord-b11d49de2b7b4836980c65505ecf2aee
出典データセット
uspto-grants-2015_09
特許番号
US09139534B2

反応ノート

読み込み中…