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Triethylamine → HCID 69060367、化合物

HRID 1821597
ノート
印刷プレビュー

反応式

HRID 1821597 の反応式
[F:1][C:2]1[CH:34]=[C:33]([F:35])[CH:32]=[CH:31][C:3]=1[O:4][C:5]1[N:10]=[C:9]2[N:11]([CH2:22][OH:23])[N:12]=[C:13]([C:14]3[CH:19]=[C:18]([F:20])[CH:17]=[CH:16][C:15]=3[F:21])[C:8]2=[C:7]([NH:24][CH2:25][CH2:26][S:27]([CH3:30])(=[O:29])=[O:28])[N:6]=1.[C:36]([NH:43][C@H:44]([C:48](O)=[O:49])[CH:45]([CH3:47])[CH3:46])([O:38][C:39]([CH3:42])([CH3:41])[CH3:40])=[O:37].CN(C1C=CC=CN=1)C.C(N(CC)CC)C.ClC(OC(C)=C)=O>C(Cl)Cl>[F:1][C:2]1[CH:34]=[C:33]([F:35])[CH:32]=[CH:31][C:3]=1[O:4][C:5]1[N:10]=[C:9]2[N:11]([CH2:22][O:23][C:48](=[O:49])[CH:44]([NH:43][C:36]([O:38][C:39]([CH3:40])([CH3:42])[CH3:41])=[O:37])[CH:45]([CH3:47])[CH3:46])[N:12]=[C:13]([C:14]3[CH:19]=[C:18]([F:20])[CH:17]=[CH:16][C:15]=3[F:21])[C:8]2=[C:7]([NH:24][CH2:25][CH2:26][S:27]([CH3:30])(=[O:28])=[O:29])[N:6]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 5

HCID 8471TriethylamineHCID 218852-DimethylaminopyridineHCID 83693Boc-L-ValineHCID 93846Isopropenyl chloroformateHCID 16117146HCID 16117146、化合物

生成物 1

HCID 69060367HCID 69060367、化合物収率 51.2%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

[6-(2,4-Difluoro-phenoxy)-3-(2,5-difluoro-phenyl)-4-(2-methanesulfonyl-ethylamino)-pyrazolo[3,4-d]pyrimidin-1-yl]-methanol (170 mg, 0.33 mmol) was dissolved in methylene chloride, and Boc-(L)-Valine (216 mg, 0.99 mmol), dimethylamino pyridine (81 mg, 0.66 mmol), and triethylamine (0.23 mL, 1.6 mmol) were added. The reaction mixture was cooled to 0° C. and stirred under nitrogen, and isopropenyl chloroformate (54 uL, 0.49 mmol) was added. The reaction mixture was stirred for 10 minutes and then partitioned between water and methylene chloride. The organic layer was washed with brine, dried (MgSO4), filtered and concentrated under reduced pressure. The residue was purified by flash chromatography through silica (1:1 hexanes/EtOAc) to give 120 mg of 2-tert-butoxycarbonylamino-3-methyl-butyric acid 6-(2,4-difluoro-phenoxy)-3-(2,5-difluoro-phenyl)-4-(2-methanesulfonyl-ethylamino)-pyrazolo[3,4-d]pyrimidin-1-ylmethyl ester as an oil.

後処理

  1. stirringThe reaction mixture was stirred for 10 minutes
  2. custompartitioned between water and methylene chloride
  3. washThe organic layer was washed with brine
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was purified by flash chromatography through silica (1:1 hexanes/EtOAc)

出典と根拠

ORDレコード
ord-83307cd99db84c60ab6e5cff4c841983
出典データセット
uspto-grants-2009_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07608603B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート