Cumylamine → HCID 57737267、化合物

HRID 549433ノート

反応式

HRID 549433 の反応式
[CH2:1]([O:3][C:4]([N:6]1[C:10]2[S:11][C:12]([C:14](O)=[O:15])=[CH:13][C:9]=2[C:8]([NH:17][C:18](=[O:33])[C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=2[NH:25][C:26]([C:28]2[NH:29][CH:30]=[CH:31][CH:32]=2)=[O:27])=[N:7]1)=[O:5])[CH3:2].F[B-](F)(F)F.N1(OC(N(C)C)=[N+](C)C)C2C=CC=CC=2N=N1.CCN(C(C)C)C(C)C.[C:65]([NH2:74])([C:68]1[CH:73]=[CH:72][CH:71]=[CH:70][CH:69]=1)([CH3:67])[CH3:66]>CN(C=O)C.CCOC(C)=O>[CH2:1]([O:3][C:4]([N:6]1[C:10]2[S:11][C:12]([C:14](=[O:15])[NH:74][C:65]([CH3:67])([C:68]3[CH:73]=[CH:72][CH:71]=[CH:70][CH:69]=3)[CH3:66])=[CH:13][C:9]=2[C:8]([NH:17][C:18](=[O:33])[C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=2[NH:25][C:26]([C:28]2[NH:29][CH:30]=[CH:31][CH:32]=2)=[O:27])=[N:7]1)=[O:5])[CH3:2]

参加物

7

反応物 4

HCID 68509CumylamineHCID 81531DiisopropylethylamineHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 57737264HCID 57737264、化合物

生成物 1

HCID 57737267HCID 57737267、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of 3-{2-[(1H-Pyrrole-2-carbonyl)-amino]-benzoylamino}-thieno[2,3-c]pyrazole-1,5-dicarboxylic acid 1-ethyl ester (198.5 mg, 0.4246 mmol), 2-(1H-benzotriazol-1-yl)-1,1,3,3-tetramethyluronium tetrafluoroborate (TBTU, 204 mg, 0.6369 mmol), DIEA (0.29 mL, 1.6984 mmol) and cumylamine (115 mg, 0.8492 mmol) in DMF (10 mL) was stirred at room temperature. After 2 hours the mixture was diluted with AcOEt (40 mL) and washed with saturated NaHCO3, water and brine. The organic layer was dried over Na2SO4 and evaporated to give 495 mg of crude that was used in the next step without further purification, LC-MS: Rt 7.36; [M+H]+ 585.

後処理

  1. washwashed with saturated NaHCO3, water and brine
  2. dry with materialThe organic layer was dried over Na2SO4
  3. customevaporated
  4. customto give 495 mg of crude that
  5. customwas used in the next step without further purification, LC-MS

出典と根拠

ORDレコード
ord-0cca8dc2289842eea1b6bd14e2ea49e5
出典データセット
uspto-grants-2011_05
特許番号
US07943654B2

反応ノート

読み込み中…