Diisopropylethylamine → HCID 89964063、化合物

HRID 2275497ノート

反応式

HRID 2275497 の反応式
[CH3:1][O:2][C:3]1[CH:7]=[C:6]([C:8]([OH:10])=O)[O:5][N:4]=1.CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.CCN(C(C)C)C(C)C.[NH2:44][C@H:45]([CH2:54][C:55]1[CH:60]=[CH:59][C:58]([C:61]2[CH:66]=[CH:65][CH:64]=[C:63]([Cl:67])[CH:62]=2)=[CH:57][CH:56]=1)[CH2:46][C@:47]([CH2:52][OH:53])([CH3:51])[C:48]([OH:50])=[O:49]>CN(C=O)C>[Cl:67][C:63]1[CH:62]=[C:61]([C:58]2[CH:57]=[CH:56][C:55]([CH2:54][C@@H:45]([NH:44][C:8]([C:6]3[O:5][N:4]=[C:3]([O:2][CH3:1])[CH:7]=3)=[O:10])[CH2:46][C@:47]([CH2:52][OH:53])([CH3:51])[C:48]([OH:50])=[O:49])=[CH:60][CH:59]=2)[CH:66]=[CH:65][CH:64]=1

参加物

6

反応物 4

HCID 81531DiisopropylethylamineHCID 3277173-Methoxy-1,2-oxazole-5-carboxylic acidHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 89964569HCID 89964569、化合物

生成物 1

HCID 89964063HCID 89964063、化合物収率 14.5%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

3-Methoxyisoxazole-5-carboxylic acid (9 mg, 32 μmol) was combined with HATU (12 mg, 32 μmol) and DMF (0.2 mL) and the resulting mixture was stirred for 5 minutes. DIPEA (17 μL, 96 μmol) and (2S,4R)-4-amino-5-(3′-chlorobiphenyl-4-yl)-2-hydroxymethyl-2-methylpentanoic acid (79 mg, 38 μmol) pre-dissolved in DMF were added and the resulting mixture was stirred for 15 minutes then concentrated. The residue was dissolved in AcOH and purified by preparative HPLC to yield the title compound (2.2 mg). MS m/z [M+H]+ calc'd for C24H25ClN2O6, 473.14. found 473.2.

後処理

  1. additionwere added
  2. stirringthe resulting mixture was stirred for 15 minutes
  3. concentrationthen concentrated
  4. dissolutionThe residue was dissolved in AcOH
  5. custompurified by preparative HPLC

出典と根拠

ORDレコード
ord-aeb65247eb694c4b87f939ff4e5a6493
出典データセット
uspto-grants-2015_09
特許番号
US09126956B2

反応ノート

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