Diisopropylethylamine → HCID 59140928、化合物

HRID 737180ノート

反応式

HRID 737180 の反応式
[CH2:1]([O:8][C:9]([N:11]1[CH2:15][CH2:14][CH2:13][CH2:12]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.CN([C:19]([O:23]N1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.CCN(C(C)C)C(C)C.[N:49]1[CH:54]=[CH:53][CH:52]=[C:51]([C:55]2[N:56]=[C:57]([NH2:60])[S:58][CH:59]=2)[CH:50]=1>CN(C=O)C>[CH2:1]([O:8][C:9]([N:11]1[CH2:15][CH2:14][CH2:13][CH:12]1[C:19](=[O:23])[NH:60][C:57]1[S:58][CH:59]=[C:55]([C:51]2[CH:50]=[N:49][CH:54]=[CH:53][CH:52]=2)[N:56]=1)=[O:10])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

6

反応物 4

HCID 81531DiisopropylethylamineHCID 1548934-(3-Pyridinyl)-2-thiazolamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 10608307Phenylmethyl 1-pyrrolidinecarboxylate

生成物 1

HCID 59140928HCID 59140928、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

Pyrrolidine-1-carboxylic acid benzyl ester, (224 mg, 0.9 mmol) was combined with 376 mg (1.0 mmol) of HATU. This mixture was dissolved in 15 ml of DMF. To this solution was added DIEA (1.8 mmol, 0.3 mL). This solution was stirred at room temperature for 1.5 hours. To this solution was then added 4-pyridin-3-yl-thiazol-2-ylamine (100 mg, 0.56 mg). Reaction mixture was stirred at room temperature overnight and then purified using reverse phase HPLC. MS: 409.1 (M+H+); H1 NMR (DMSO-d6): δ(ppm) (HCl salt) 12.62 (s, 1H), 9.28 (s, 1H), 8.78 (s, 1H), 8.03 (m, 2H), 7.38 (m, 3H), 7.04 (d, 2H), 5.00 (m, 2H), 4.53 (m, 1H), 3.62 (m, 2H), 2.22 (m, 1H), 1.89 (m, 4H).

後処理

  1. customReaction mixture
  2. stirringwas stirred at room temperature overnight
  3. custompurified

出典と根拠

ORDレコード
ord-8d20a0ced70d470d87e668b52970f89b
出典データセット
uspto-grants-2009_09
特許番号
US07595398B2

反応ノート

読み込み中…