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Water → HCID 59507059、化合物

HRID 1800508
ノート
印刷プレビュー

反応式

HRID 1800508 の反応式
[F:1][C:2]([F:16])([O:6][C:7]1[CH:8]=[C:9]([CH:13]=[CH:14][CH:15]=1)[C:10]([OH:12])=O)[CH:3]([F:5])[F:4].F[P-](F)(F)(F)(F)F.N1(OC(N(C)C)=[N+](C)C)C2N=CC=CC=2N=N1.[NH2:41][C:42]1[CH:43]=[CH:44][C:45]([CH3:64])=[C:46]([CH:63]=1)[O:47][C:48]1[N:53]=[C:52]2[S:54][C:55]([NH:57][C:58]([CH:60]3[CH2:62][CH2:61]3)=[O:59])=[N:56][C:51]2=[CH:50][CH:49]=1.O>N1C=CC=CC=1>[CH:60]1([C:58]([NH:57][C:55]2[S:54][C:52]3[C:51]([N:56]=2)=[CH:50][CH:49]=[C:48]([O:47][C:46]2[CH:63]=[C:42]([NH:41][C:10](=[O:12])[C:9]4[CH:13]=[CH:14][CH:15]=[C:7]([O:6][C:2]([F:1])([F:16])[CH:3]([F:4])[F:5])[CH:8]=4)[CH:43]=[CH:44][C:45]=2[CH3:64])[N:53]=3)=[O:59])[CH2:61][CH2:62]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 5786803-(1,1,2,2-Tetrafluoroethoxy)benzoic acidHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 58451281HCID 58451281、化合物

生成物 1

HCID 59507059HCID 59507059、化合物収率 56%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

To a solution of 3-(1,1,2,2-tetrafluoroethoxy)benzoic acid (44 mg, 0.185 mmol) in pyridine (2.0 mL) was added O-(7-azabenzotriazol-1-yl)-N,N,N′,N′-tetramethyluronium hexafluorophosphate (70 mg, 0.185 mmol), and the mixture was stirred at room temperature for 10 min. N-[5-(5-Amino-2-methylphenoxy)[1,3]thiazolo[5,4-b]pyridin-2-yl]cyclopropanecarboxamide (60 mg, 0.176 mmol) produced in Example C47(i) was added to the obtained solution, and the mixture was stirred at 70° C. for 20 hr. After the reaction mixture was cooled to room temperature, water (2 mL) was added, and the obtained precipitate was collected by filtration, washed with water and ethyl acetate, and dried to give the title compound (55 mg, 56%) as a colorless powder.

後処理

  1. additionwas added to the obtained solution
  2. stirringthe mixture was stirred at 70° C. for 20 hr
  3. temperatureAfter the reaction mixture was cooled to room temperature
  4. filtrationthe obtained precipitate was collected by filtration
  5. washwashed with water and ethyl acetate
  6. customdried

出典と根拠

ORDレコード
ord-9afbb5edb39a44308f7418eb2d25402e
出典データセット
uspto-grants-2013_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08344135B2

反応ノート

読み込み中…

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