Aminotetrazole → HCID 178520732、化合物

HRID 220150

反応式

HRID 220150 の反応式
[F:1][C:2]([F:25])([F:24])[C:3]1[NH:7][N:6]=[C:5]([C:8]2[CH:13]=[CH:12][C:11]([C@H:14]3[CH2:19][CH2:18][C@H:17]([CH2:20][C:21]([OH:23])=O)[CH2:16][CH2:15]3)=[CH:10][CH:9]=2)[CH:4]=1.[N:26]1[NH:27][N:28]=[N:29][C:30]=1[NH2:31].F[P-](F)(F)(F)(F)F.N1(OC(N(C)C)=[N+](C)C)C2N=CC=CC=2N=N1.C(N(C(C)C)CC)(C)C>CN(C)C=O>[N:26]1[NH:27][N:28]=[N:29][C:30]=1[NH:31][C:21](=[O:23])[CH2:20][C@H:17]1[CH2:16][CH2:15][C@H:14]([C:11]2[CH:12]=[CH:13][C:8]([C:5]3[CH:4]=[C:3]([C:2]([F:24])([F:1])[F:25])[NH:7][N:6]=3)=[CH:9][CH:10]=2)[CH2:19][CH2:18]1

参加物

6

反応物 4

HCID 20467AminotetrazoleHCID 81531DiisopropylethylamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 178525542HCID 178525542、化合物

生成物 1

HCID 178520732HCID 178520732、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a 20 mL scintillation vial was added the product from Example 28 (30 mg, 0.085 mmol), 2H-tetrazol-5-amine (8.00 mg, 0.088 mmol) and N,N-dimethylformamide (0.85 mL) followed by O-(7-azabenzotriazol-1-yl)-N,N,N′,N′-tetramethyluronium hexafluorophosphate (39.0 mg, 0.102 mmol) and diisopropylethylamine (30 μL, 0.176 mmol). Following 4 hours of stirring, the solvent was evaporated and the residue purified over RP-HPLC to afford the title product. 1H NMR (500 MHz, DMSO-d6) δ ppm 1.06-1.26 (m, 2 H), 1.43-1.57 (m, 2 H), 1.76-1.92 (m, 5 H), 2.36-2.41 (m, 2 H), 6.96-7.23 (m, 1 H), 7.23-7.46 (m, 2 H), 7.57-7.80 (m, 2 H), 11.99 (s, 1 H), 13.98 (s, 1 H), 15.83 (s, 1 H); MS (ESI) m/z 420 [M+H]+.

後処理

  1. customthe solvent was evaporated
  2. customthe residue purified over RP-HPLC

出典と根拠

ORDレコード
ord-6c465b34c9a4464cafa074579f8fb490
出典データセット
uspto-grants-2012_06
特許番号
US08202878B2

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