4-Methylmorpholine → HCID 178487704, 화합물

HRID 2044020노트

반응식

HRID 2044020 반응식
[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]

참가 물질

6

반응물 4

HCID 79724-MethylmorpholineHCID 25517Ammonium Chloride2회HCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 178487707HCID 178487707, 화합물

생성물 1

HCID 178487704HCID 178487704, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-c757f5ea7257429794f94baf93d54080
출처 데이터셋
uspto-grants-2013_11
특허 번호
US08586744B2

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