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Diisopropylethylamine → HCID 57033673、化合物

HRID 1250868
ノート
印刷プレビュー

反応式

HRID 1250868 の反応式
[C:1]([O:5][C:6]([C@@H:8]([NH:23][S:24]([C:27]1[CH:32]=[CH:31][C:30]([C:33]([F:36])([F:35])[F:34])=[CH:29][CH:28]=1)(=[O:26])=[O:25])[CH2:9][C:10]1[CH:22]=[CH:21][C:13]([O:14][CH2:15][CH2:16][CH2:17][C:18](O)=[O:19])=[CH:12][CH:11]=1)=[O:7])([CH3:4])([CH3:3])[CH3:2].C([N:40](C(C)C)CC)(C)C.CN(C(O[N:54]1N=NC2[CH:57]=[CH:58][CH:59]=[N:60][C:55]1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F>O1CCCC1.N1CCCN=C1N>[C:1]([O:5][C:6](=[O:7])[C@@H:8]([NH:23][S:24]([C:27]1[CH:28]=[CH:29][C:30]([C:33]([F:34])([F:35])[F:36])=[CH:31][CH:32]=1)(=[O:25])=[O:26])[CH2:9][C:10]1[CH:11]=[CH:12][C:13]([O:14][CH2:15][CH2:16][CH2:17][C:18](=[O:19])[NH:40][C:55]2[NH:54][CH2:57][CH2:58][CH2:59][N:60]=2)=[CH:21][CH:22]=1)([CH3:2])([CH3:3])[CH3:4]
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 3

HCID 81531DiisopropylethylamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 69922482HCID 69922482、化合物

生成物 1

HCID 57033673HCID 57033673、化合物

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒
HCID 3287412
1,4,5,6-Tetrahydropyrimidin-2-amine
溶媒

実験手順

56 mg of 4-{4-[(2S)-2-tert-butoxycarbonyl-2-(4-trifluoromethylbenzenesulfonylamino)-ethyl]-phenoxy}-butyric acid were dissolved in tetrahydrofuran and 12.5 mg of 1,4,5,6-tetrahydropyrimidin-2-ylamine, 68 mg of diisopropylethylamine and 44 mg of HATU were added. The reaction mixture was stirred overnight, and the solvent was removed in vacuo. The residue was dissolved in dichloromethane and washed with saturated aqueous sodium bicarbonate solution and saturated aqueous sodium chloride solution. The organic phase was dried with sodium sulfate, filtered and the solvent was removed in vacuo. The residue was chromatographed on reversed-phase (C-18) silica gel eluting with a gradient of 10-90% acetonitrile in water. Yield 37.3 mg. MS (FAB+): m/e=613.3 (M+H)+.

後処理

  1. customthe solvent was removed in vacuo
  2. dissolutionThe residue was dissolved in dichloromethane
  3. washwashed with saturated aqueous sodium bicarbonate solution and saturated aqueous sodium chloride solution
  4. dry with materialThe organic phase was dried with sodium sulfate
  5. filtrationfiltered
  6. customthe solvent was removed in vacuo
  7. customThe residue was chromatographed on reversed-phase (C-18) silica gel eluting with a gradient of 10-90% acetonitrile in water

出典と根拠

ORDレコード
ord-88afa19c42ee4650b8c5a96022b8b6bb
出典データセット
uspto-grants-2002_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06340679B1

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート