Water → HCID 86593419, 화합물

HRID 1247847노트

반응식

HRID 1247847 반응식
[NH2:1][C:2]1[N:6]([CH2:7][CH2:8][F:9])[N:5]=[CH:4][C:3]=1[NH:10][C:11](=[O:22])[CH2:12][CH2:13][NH:14][C:15](=[O:21])[O:16][C:17]([CH3:20])([CH3:19])[CH3:18].C(N(CC)CC)C.[C:30](Cl)([C:43]1[CH:48]=[CH:47][CH:46]=[CH:45][CH:44]=1)([C:37]1[CH:42]=[CH:41][CH:40]=[CH:39][CH:38]=1)[C:31]1[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1.O>CN(C)C=O.CN(C)C1C=CN=CC=1>[F:9][CH2:8][CH2:7][N:6]1[C:2]([NH:1][C:30]([C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)([C:43]2[CH:44]=[CH:45][CH:46]=[CH:47][CH:48]=2)[C:37]2[CH:38]=[CH:39][CH:40]=[CH:41][CH:42]=2)=[C:3]([NH:10][C:11](=[O:22])[CH2:12][CH2:13][NH:14][C:15](=[O:21])[O:16][C:17]([CH3:19])([CH3:18])[CH3:20])[CH:4]=[N:5]1

참가 물질

7

반응물 4

HCID 962WaterHCID 6456Trityl chlorideHCID 8471TriethylamineHCID 86593418HCID 86593418, 화합물

생성물 1

HCID 86593419HCID 86593419, 화합물수율 49.2%

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6228Dimethylformamide용매

실험 절차

To a solution of tert-butyl (3-{[5-amino-1-(2-fluoroethyl)-1H-pyrazol-4-yl]amino}-3-oxopropyl)carbamate (2.3 g) in N,N-dimethylformamide (12 ml) were added triethylamine (1.48 g), 4-dimethylaminopyridine (35.6 mg) and trityl chloride (2.2 g) at room temperature. The reaction mixture was stirred for 2 hours, and water was added. The mixture was extracted with ethyl acetate, and the organic layer was washed with water and aqueous sodium chloride solution. The organic layer was dried over magnesium sulfate and concentrated in vacuo. Acetonitrile was added, and the precipitate was collected by filtration to give tert-butyl (3-{[1-(2-fluoroethyl)-5-(tritylamino)-1H-pyrazol-4-yl]amino}-3-oxopropyl)carbamate (2 g).

후처리

  1. extractionThe mixture was extracted with ethyl acetate
  2. washthe organic layer was washed with water and aqueous sodium chloride solution
  3. dry with materialThe organic layer was dried over magnesium sulfate
  4. concentrationconcentrated in vacuo
  5. additionAcetonitrile was added
  6. filtrationthe precipitate was collected by filtration

출처 및 근거

ORD 기록
ord-9ead8a85dc9547ce8bf9d5cf91bdf0e7
출처 데이터셋
uspto-grants-2006_10
특허 번호
US07129232B2

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