4-Methylmorpholine → HCID 178487704、化合物

HRID 2044020ノート

反応式

HRID 2044020 の反応式
[Cl:1][C:2]1[C:3]([O:16][CH3:17])=[CH:4][CH:5]=[C:6]2[C:11]=1[N:10]=[C:9]([C:12](O)=[O:13])[CH:8]=[C:7]2[OH:15].[Cl-].[NH4+].C[N:21](C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.CN1CCOCC1>CN(C=O)C>[Cl:1][C:2]1[C:3]([O:16][CH3:17])=[CH:4][CH:5]=[C:6]2[C:11]=1[N:10]=[C:9]([C:12]([NH2:21])=[O:13])[CH:8]=[C:7]2[OH:15]

参加物

6

反応物 4

HCID 79724-MethylmorpholineHCID 25517Ammonium Chloride2 回HCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 178487707HCID 178487707、化合物

生成物 1

HCID 178487704HCID 178487704、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

8-Chloro-4-hydroxy-7-methoxy-quinoline-2-carboxylic acid (115 mg, 0.45 mmol) and ammoniumchloride (36 mg, 0.68 mmol) were dissolved in DMF (4 mL). HATU (342 mg, 0.9 mmol) and NMM (159 mg, 1.58 mmol) were added and the mixture was stirred at r.t. overnight. An additional amount of ammoniumchloride (72 mg, 13.5 mmol) was added and heated to 53° C. for 18 h. The reaction mixture was cooled to r.t. and concentrated to give 8-chloro-4-hydroxy-7-methoxy-quinoline-2-carboxylic acid amide as a yellow solid.

後処理

  1. temperatureheated to 53° C. for 18 h
  2. temperatureThe reaction mixture was cooled to r.t.
  3. concentrationconcentrated

出典と根拠

ORDレコード
ord-c757f5ea7257429794f94baf93d54080
出典データセット
uspto-grants-2013_11
特許番号
US08586744B2

反応ノート

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