Anthranilamide → HCID 57737846、化合物

HRID 598422ノート

反応式

HRID 598422 の反応式
[Br:1][C:2]1[S:3][CH:4]=[C:5]([C:7]([OH:9])=O)[N:6]=1.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.[NH2:34][C:35]1[CH:43]=[CH:42][CH:41]=[CH:40][C:36]=1[C:37]([NH2:39])=[O:38].C(N(CC)C(C)C)(C)C>CN(C)C=O>[NH2:39][C:37]([C:36]1[CH:40]=[CH:41][CH:42]=[CH:43][C:35]=1[NH:34][C:7]([C:5]1[N:6]=[C:2]([Br:1])[S:3][CH:4]=1)=[O:9])=[O:38]

参加物

6

反応物 4

HCID 6942AnthranilamideHCID 81531DiisopropylethylamineHCID 27632092-Bromo-1,3-thiazole-4-carboxylic acidHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)

生成物 1

HCID 57737846HCID 57737846、化合物収率 89.9%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

2-Bromo-4-thiazolecarboxylic acid (1 g), HATU (2.01 g) and 2-aminobenzamide (0.65 g) are introduced into N,N-dimethylformamide (DMF) (20 ml). The mixture is cooled with an ice bath, and N,N-diisopropylethylamine (0.90 ml) is added. The reaction mixture is stirred at room temperature for 6 days, poured into ice-water and allowed to thaw with stirring, and the precipitated solid is filtered off with suction, washed twice with water, twice with diethyl ether and dried in vacuo. Intermediate III.2 is obtained as a solid (1.4 g).

後処理

  1. temperatureThe mixture is cooled with an ice bath
  2. stirringwith stirring
  3. filtrationthe precipitated solid is filtered off with suction
  4. washwashed twice with water, twice with diethyl ether
  5. customdried in vacuo

出典と根拠

ORDレコード
ord-77731f6d97124e189f08fdc3451fd289
出典データセット
uspto-grants-2011_03
特許番号
US07897626B2

反応ノート

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