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Diisopropylethylamine → HCID 58413247、化合物

HRID 532304
ノート
印刷プレビュー

反応式

HRID 532304 の反応式
C[N:2](C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.[CH:25]([O:28][C:29]1[C:34]([NH:35][C:36]2[C:37]3[C:44]([CH3:45])=[C:43]([C:46]([OH:48])=O)[S:42][C:38]=3[N:39]=[CH:40][N:41]=2)=[CH:33][CH:32]=[CH:31][N:30]=1)([CH3:27])[CH3:26].CCN(C(C)C)C(C)C.N.CO>CN(C=O)C.CCOC(C)=O>[CH:25]([O:28][C:29]1[C:34]([NH:35][C:36]2[C:37]3[C:44]([CH3:45])=[C:43]([C:46]([NH2:2])=[O:48])[S:42][C:38]=3[N:39]=[CH:40][N:41]=2)=[CH:33][CH:32]=[CH:31][N:30]=1)([CH3:26])[CH3:27]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

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 21705897Ammonia methanolHCID 46182084HCID 46182084、化合物

生成物 1

HCID 58413247HCID 58413247、化合物

試薬・触媒・溶媒 2

HCID 6228
Dimethylformamide
溶媒
HCID 8857Ethyl Acetate溶媒

反応条件

温度
0 °C

実験手順

HATU (182.0 mg) was added to an ice cooled solution of 150 mg 4-(2-Isopropoxypyridin-3-ylamino)-5-methyl-thieno[2,3-d]pyrimidine-6-carboxylic acid and DIPEA (83.0 μl) in DMF (3.0 ml). The mixture was stirred at 0° C. for 20 min then ammonia/MeOH (7M; 1.5 ml) was added and it was allowed to warm to room temperature overnight. The mixture was diluted with EtOAc and washed with water, 2M NaOH and concentrated in vacuo. The residue was triturated with Et2O and filtered to give the title compound.

後処理

  1. temperatureto warm to room temperature overnight
  2. washwashed with water, 2M NaOH
  3. concentrationconcentrated in vacuo
  4. customThe residue was triturated with Et2O
  5. filtrationfiltered

出典と根拠

ORDレコード
ord-671b82b60ff343478a1df6fcbb4a7e4d
出典データセット
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08853193B2

反応ノート

読み込み中…

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