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3,4-Dichloro-5-isothiazolecarboxylic acid → 3,4-Dichloroisothiazole-5-carboxylic acid [5-fluoro-2-(4-fluorobenzyloxy)pyrimidin-4-yl]amide

HRID 1500013
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HRID 1500013 반응식
[Cl:1][C:2]1[C:6]([Cl:7])=[C:5]([C:8]([OH:10])=O)[S:4][N:3]=1.[F:11][C:12]1[C:13]([NH2:27])=[N:14][C:15]([O:18][CH2:19][C:20]2[CH:25]=[CH:24][C:23]([F:26])=[CH:22][CH:21]=2)=[N:16][CH:17]=1.[Li+].C[Si]([N-][Si](C)(C)C)(C)C.ClN1C(Cl)=C(C(Cl)=O)SC1>C(Cl)(=O)C(Cl)=O.CN(C)C=O.C1COCC1.O>[F:11][C:12]1[C:13]([NH:27][C:8]([C:5]2[S:4][N:3]=[C:2]([Cl:1])[C:6]=2[Cl:7])=[O:10])=[N:14][C:15]([O:18][CH2:19][C:20]2[CH:21]=[CH:22][C:23]([F:26])=[CH:24][CH:25]=2)=[N:16][CH:17]=1
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참가 물질

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HCID 498373,4-Dichloro-5-isothiazolecarboxylic acidHCID 2733832Lithium hexamethyldisilazaneHCID 578185745-Fluoro-2-(4-fluorobenzyloxy)pyrimidin-4-amineHCID 866332223,4-Dichlorothiazole-5-carbonyl chloride

생성물 1

HCID 578192363,4-Dichloroisothiazole-5-carboxylic acid [5-fluoro-2-(4-fluorobenzyloxy)pyrimidin-4-yl]amide수율 12.3%

시약·촉매·용매

4
HCID 6228Dimethylformamide촉매HCID 962Water용매HCID 8028Tetrahydrofuran용매2회HCID 65578Oxalyl chloride용매

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온도
80 °C

실험 절차

To a suspension of 3,4-dichloroisothiazole-5-carboxylic acid (0.15 g, 0.76 mmol) in oxalyl chloride (2 mL) was added a catalytic amount of dimethylformamide (2 drops) and the mixture was heated to 80° C. and stirred for 2 h. The excess oxalyl chloride was removed on the rotary evaporator. Meanwhile, 5-fluoro-2-(4-fluorobenzyloxy)-pyrimidin-4-ylamine (0.17 g, 0.68 mmol) was dissolved in THF (1 mL), treated with LiHMDS (1M in THF, 0.76 mL, 0.76 mmol) and stirred for 10 min. The freshly prepared 3,4-dichlorothiazole-5-carbonyl chloride*, dissolved in THF (1 mL), was added and the reaction was capped and stirred for 12 h. The reaction was diluted with water and the target compound was extracted with CH2Cl2 (3×5 mL). The combined extracts were dried over MgSO4 and then evaporated under reduced pressure. The mixture was eluted with CH2Cl2 through an anionic-exchange solid phase extraction column and then further purified by reverse-phase chromatography to give 3,4-dichloroisothiazole-5-carboxylic acid [5-fluoro-2-(4-fluorobenzyloxy)pyrimidin-4-yl]amide (0.035 g, 12%) as a tan solid: mp 87-90° C.; 1H NMR (400 MHz, DMSO-d6) δ 11.78 (s, 1H), 8.67 (s, 1H), 7.51-7.48 (m, 2H), 7.24-7.19 (m, 2H), 5.25 (s, 2H); MS (ESI) m/z 417 (M+H)+, 415 (M−H)−. *Nagata, T.; Kogure, A.; Yonekura, N.; Hanai, R.; Kaneko, I.; Nakano, Y. JP 2007211002 A

후처리

  1. customThe excess oxalyl chloride was removed on the rotary evaporator
  2. stirringstirred for 10 min
  3. additionwas added
  4. customthe reaction was capped
  5. stirringstirred for 12 h
  6. extractionthe target compound was extracted with CH2Cl2 (3×5 mL)
  7. dry with materialThe combined extracts were dried over MgSO4
  8. customevaporated under reduced pressure
  9. washThe mixture was eluted with CH2Cl2 through an anionic-exchange solid phase extraction column
  10. customfurther purified by reverse-phase chromatography

출처 및 근거

ORD 기록
ord-16d4dd5ada8044129114c22da02ec662
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09204653B2

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