Diisopropylethylamine → HCID 57512966、化合物

HRID 14190ノート

反応式

HRID 14190 の反応式
[CH2:1]([N:5]1[C:10]2[CH:11]=[C:12]([C:20](O)=[O:21])[CH:13]=[C:14]([C:15]3[O:16][CH:17]=[CH:18][N:19]=3)[C:9]=2[O:8][CH2:7][CH2:6]1)[CH2:2][CH2:3][CH3:4].CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.C(N(C(C)C)CC)(C)C.[NH2:56][C@@H:57]([CH2:71][C:72]1[CH:77]=[C:76]([F:78])[CH:75]=[C:74]([F:79])[CH:73]=1)[C@H:58]([OH:70])[CH2:59][NH:60][CH2:61][C:62]1[CH:67]=[CH:66][CH:65]=[C:64]([CH2:68][CH3:69])[CH:63]=1>C(Cl)Cl>[CH2:1]([N:5]1[C:10]2[CH:11]=[C:12]([C:20]([NH:56][C@@H:57]([CH2:71][C:72]3[CH:73]=[C:74]([F:79])[CH:75]=[C:76]([F:78])[CH:77]=3)[C@H:58]([OH:70])[CH2:59][NH:60][CH2:61][C:62]3[CH:67]=[CH:66][CH:65]=[C:64]([CH2:68][CH3:69])[CH:63]=3)=[O:21])[CH:13]=[C:14]([C:15]3[O:16][CH:17]=[CH:18][N:19]=3)[C:9]=2[O:8][CH2:7][CH2:6]1)[CH2:2][CH2:3][CH3:4]

参加物

6

反応物 4

HCID 81531DiisopropylethylamineHCID 2733084Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 210859304-Butyl-8-(1,3-oxazol-2-yl)-3,4-dihydro-2H-1,4-benzoxazine-6-carboxylic acidHCID 57487282(2R,3S)-3-amino-4-(3,5-difluorophenyl)-1-[(3-ethylbenzyl)amino]butan-2-ol

生成物 1

HCID 57512966HCID 57512966、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A solution of 4-Butyl-8-(1,3-oxazol-2-yl)-3,4-dihydro-2H-1,4-benzoxazine-6-carboxylic acid (450 mg, HBTU (853 mg), and diisopropylethylamine (580 mg) was stirred in methylene chloride (15 mL) for 15 min. A solution of (2R,3S)-3-amino-4-(3,5-difluorophenyl)-1-[(3-ethylbenzyl)amino]butan-2-ol (606 mg) in methylene chloride (7 mL) was added and the reaction mixture was stirred overnight. The mixture was filtered with methylene chloride, dried (magnesium sulfate), and concentrated under reduced pressure. Purification by flash column chromatography (silica, 1:9 methanol/chloroform) provided 400 mg of the title compound: ESI MS m/z 619 [M+H]+.

後処理

  1. filtrationThe mixture was filtered with methylene chloride
  2. dry with materialdried (magnesium sulfate)
  3. concentrationconcentrated under reduced pressure
  4. customPurification by flash column chromatography (silica, 1:9 methanol/chloroform)

出典と根拠

ORDレコード
ord-9df640648daf4f96afe2372956fbc8da
出典データセット
uspto-grants-2010_06
特許番号
US07727997B2

反応ノート

読み込み中…