4-Methylmorpholine → HCID 178487704、化合物

HRID 1367734ノート

反応式

HRID 1367734 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-3afba60a7d964b95b7686065f50ad4e7
出典データセット
uspto-grants-2011_02
特許番号
US07893264B2

反応ノート

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