Diisopropylethylamine → HCID 67281619、化合物

HRID 446964

反応式

HRID 446964 の反応式
[C:1]([O:5][C:6]([N:8]([CH3:38])[CH:9]([CH3:37])[C:10]([NH:12][CH:13]([CH:31]1[CH2:36][CH2:35][CH2:34][CH2:33][CH2:32]1)[C:14]([N:16]1[CH:23]2[CH:19]([N:20]([S:27]([CH3:30])(=[O:29])=[O:28])[CH2:21][CH:22]2[C:24]([OH:26])=O)[CH2:18][CH2:17]1)=[O:15])=[O:11])=[O:7])([CH3:4])([CH3:3])[CH3:2].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.[C@H:72]1([NH2:82])[C:81]2[C:76](=[CH:77][CH:78]=[CH:79][CH:80]=2)[CH2:75][CH2:74][CH2:73]1>CN1C(=O)CCC1.CCOC(C)=O>[C:1]([O:5][C:6](=[O:7])[N:8]([CH:9]([C:10](=[O:11])[NH:12][CH:13]([CH:31]1[CH2:32][CH2:33][CH2:34][CH2:35][CH2:36]1)[C:14]([N:16]1[CH2:17][CH2:18][CH:19]2[N:20]([S:27]([CH3:30])(=[O:28])=[O:29])[CH2:21][CH:22]([C:24](=[O:26])[NH:82][CH:72]3[C:81]4[C:76](=[CH:77][CH:78]=[CH:79][CH:80]=4)[CH2:75][CH2:74][CH2:73]3)[CH:23]12)=[O:15])[CH3:37])[CH3:38])([CH3:2])([CH3:4])[CH3:3]

参加物

7

反応物 4

HCID 81531DiisopropylethylamineHCID 70580721-Aminotetralin, (R)-HCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 672809014-{2-[2-(tert-Butoxycarbonyl-methyl-amino)-propionylamino]-2-cyclohexyl-acetyl}-1-methanesulfonyl-octahydro-pyrrolo[3,2-b]pyrrole-3-carboxylic acid

生成物 1

HCID 67281619HCID 67281619、化合物

試薬・触媒・溶媒 2

HCID 8857Ethyl Acetate溶媒HCID 13387N-methyl-2-pyrrolidone溶媒2 回

実験手順

A solution of crude 21 (106 mg, 0.19 mmol) in NMP (5 mL) was cooled to 0° C. and treated with HATU (73 mg, 0.19 mmol) and DIPEA (0.1 mL, 0.57 mmol). After 10 min, (1R)-1,2,3,4-tetrahydro-naphthalen-1-ylamine (0.05 mL, 0.35 mmol) in NMP (3 mL) was added. The reaction was allowed to warm to ambient temperature. After 16 h, the solution was diluted with EtOAc, washed successively with 1M HCl, brine, dried over anhydrous Na2SO4, filtered and concentrated to afford 22 which was used without further purification. Mass spectrum, m/z [688.5] (M+H)+.

後処理

  1. waitAfter 16 h
  2. washwashed successively with 1M HCl, brine
  3. dry with materialdried over anhydrous Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-b3daea1956ff4f86bf1584ccf8fb951d
出典データセット
uspto-grants-2013_07
特許番号
US08481495B2

関連ノート

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