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1-Hydroxy-2-naphthoic acid → HCID 58865449、化合物

HRID 1354836
ノート
印刷プレビュー

反応式

HRID 1354836 の反応式
[OH:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH:5]=[CH:4][C:3]=1[C:12]([OH:14])=O.CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.C(N(C(C)C)C(C)C)C.[NH2:48][C:49]1[CH:111]=[CH:110][C:52]([C:53]([NH:55][C:56]2[CH:57]=[C:58]3[C:63](=[CH:64][CH:65]=2)[N:62]=[C:61]([N:66]2[CH2:71][C@@H:70]([NH:72][C:73]([O:75][C:76]([CH3:79])([CH3:78])[CH3:77])=[O:74])[CH2:69][C@@H:68]([NH:80][C:81]([O:83][C:84]([CH3:87])([CH3:86])[CH3:85])=[O:82])[CH2:67]2)[C:60]([N:88]2[CH2:93][C@@H:92]([NH:94][C:95]([O:97][C:98]([CH3:101])([CH3:100])[CH3:99])=[O:96])[CH2:91][C@@H:90]([NH:102][C:103]([O:105][C:106]([CH3:109])([CH3:108])[CH3:107])=[O:104])[CH2:89]2)=[N:59]3)=[O:54])=[CH:51][CH:50]=1>CN(C=O)C.CCOC(C)=O>[C:76]([O:75][C:73]([NH:72][C@@H:70]1[CH2:69][C@H:68]([NH:80][C:81]([O:83][C:84]([CH3:85])([CH3:86])[CH3:87])=[O:82])[CH2:67][N:66]([C:61]2[C:60]([N:88]3[CH2:93][C@@H:92]([NH:94][C:95]([O:97][C:98]([CH3:101])([CH3:100])[CH3:99])=[O:96])[CH2:91][C@@H:90]([NH:102][C:103]([O:105][C:106]([CH3:108])([CH3:107])[CH3:109])=[O:104])[CH2:89]3)=[N:59][C:58]3[C:63](=[CH:64][CH:65]=[C:56]([NH:55][C:53]([C:52]4[CH:110]=[CH:111][C:49]([NH:48][C:12]([C:3]5[CH:4]=[CH:5][C:6]6[C:11](=[CH:10][CH:9]=[CH:8][CH:7]=6)[C:2]=5[OH:1])=[O:14])=[CH:50][CH:51]=4)=[O:54])[CH:57]=3)[N:62]=2)[CH2:71]1)=[O:74])([CH3:77])([CH3:78])[CH3:79]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 68441-Hydroxy-2-naphthoic acidHCID 81531DiisopropylethylamineHCID 2733084Methanaminium, N-((1H-benzotriazol-1-yloxy)(dimethylamino)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 58865803HCID 58865803、化合物

生成物 1

HCID 58865449HCID 58865449、化合物収率 12.5%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

1-Hydroxy-naphthalene-2-carboxylic acid (142) (0.016 g, 0.085 mmol) was dissolved in DMF (0.8 mL) and HBTU (0.032 g, 0.085 mmol) followed by iPr2EtN (0.022 mL, 0.128 mmol) were added. The mixture was shaken at room temperature for 25 minutes. 4-Amino-N-(2,3-bis-((3R,5S)-3,5-bis-(tert-Butoxycarbonylamino)-piperidin-1-yl)-quinoxalin-6-yl)-benzamide (252) (0.06 g, 0.068 mmol) was added and the mixture was shaken at room temperature for 16 h. The mixture was diluted with EtOAc, washed with sodium bicarbonate and brine via extraction, dried over MgSO4 and concentrated under reduced pressure. Purification by flash chromatography on silica gel using a gradient of hexane and EtOAc gave the desired product (253) (0.009 g, 0.0085 mmol, 12.5% yield). LC-MS (ESI): (exact mass: 1060.54, mol. wt: 1061.23) m/e=1062.0 [M+1]+.

後処理

  1. additionwere added
  2. stirringthe mixture was shaken at room temperature for 16 h
  3. washwashed with sodium bicarbonate and brine via extraction
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated under reduced pressure
  6. customPurification by flash chromatography on silica gel using a gradient of hexane and EtOAc

出典と根拠

ORDレコード
ord-d24b2a7fa96f4fee933eedd61e21dce8
出典データセット
uspto-grants-2007_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07223759B2

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