Diisopropylethylamine → tert-butyl-N-{1-[(6-amino-4-chloropyridin-2-yl)carbamoyl]ethyl}carbamate

HRID 1772164

反応式

HRID 1772164 の反応式
CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.[C:25]([O:29][C:30]([NH:32][CH:33]([CH3:37])[C:34]([OH:36])=O)=[O:31])([CH3:28])([CH3:27])[CH3:26].[Cl:38][C:39]1[CH:44]=[C:43]([NH2:45])[N:42]=[C:41]([NH2:46])[CH:40]=1.CCN(C(C)C)C(C)C>CN1C(=O)CCC1>[C:25]([O:29][C:30](=[O:31])[NH:32][CH:33]([C:34](=[O:36])[NH:46][C:41]1[CH:40]=[C:39]([Cl:38])[CH:44]=[C:43]([NH2:45])[N:42]=1)[CH3:37])([CH3:26])([CH3:27])[CH3:28]

参加物

6

反応物 4

HCID 81531DiisopropylethylamineHCID 2378474-Chloropyridine-2,6-diamineHCID 2684712-N-Boc-aminopropionic 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 117903116tert-butyl-N-{1-[(6-amino-4-chloropyridin-2-yl)carbamoyl]ethyl}carbamate

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒

実験手順

HATU (2.7 g, 7.1 mmol) is added to a mixture of 2-{[(tert-butoxy)carbonyl]amino}-propanoic acid (850 mg, 4.5 mmol), 4-chloropyridine-2,6-diamine (1 g, 7.0 mmol), DIPEA (4.6 ml, 26.5 mmol) and NMP (7 ml) and the mixture is stirred at RT for 18 h. The mixture is concentrated in vacuo and the product purified by RP HPLC. Yield: 770 mg (55%). HPLC-MS: M+H=315 (Method—2).

後処理

  1. concentrationThe mixture is concentrated in vacuo
  2. customthe product purified by RP HPLC

出典と根拠

ORDレコード
ord-84646cea1bb54e5da6bbe6b6fb421cdc
出典データセット
uspto-grants-2016_02
特許番号
US09249151B2

関連ノート

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