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2-Methoxyethanol → tert-Butyl 2-(2-amino-6,7-dihydro-5H-benzo[6,7]cyclohepta[1,2-d]pyrimidin-4-yl)octahydro-5H-pyrrolo[3,4-c]pyridine-5-carboxylate

HRID 1027888
ノート
印刷プレビュー

反応式

HRID 1027888 の反応式
Cl[C:2]1[C:3]2[CH2:13][CH2:12][CH2:11][C:10]3[CH:14]=[CH:15][CH:16]=[CH:17][C:9]=3[C:4]=2[N:5]=[C:6]([NH2:8])[N:7]=1.[CH2:18]1[CH:26]2[CH:21]([CH2:22][N:23]([C:27]([O:29][C:30]([CH3:33])([CH3:32])[CH3:31])=[O:28])[CH2:24][CH2:25]2)[CH2:20][NH:19]1.COCCO.C(N(CC)C(C)C)(C)C>C(Cl)Cl>[NH2:8][C:6]1[N:7]=[C:2]([N:19]2[CH2:18][CH:26]3[CH:21]([CH2:22][N:23]([C:27]([O:29][C:30]([CH3:33])([CH3:32])[CH3:31])=[O:28])[CH2:24][CH2:25]3)[CH2:20]2)[C:3]2[CH2:13][CH2:12][CH2:11][C:10]3[CH:14]=[CH:15][CH:16]=[CH:17][C:9]=3[C:4]=2[N:5]=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

6

反応物 4

HCID 80192-MethoxyethanolHCID 81531DiisopropylethylamineHCID 19691292tert-Butyl octahydro-5H-pyrrolo(3,4-c)pyridine-5-carboxylateHCID 866218984-chloro-6,7-dihydro-5H-benzo[6,7]cyclohepta[1,2-d]pyrimidin-2-amine

生成物 1

HCID 86621897tert-Butyl 2-(2-amino-6,7-dihydro-5H-benzo[6,7]cyclohepta[1,2-d]pyrimidin-4-yl)octahydro-5H-pyrrolo[3,4-c]pyridine-5-carboxylate

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
115 °C

実験手順

The product from Example 68A (40 mg, 0.16 mmol) was mixed with tert-butyl hexahydro-1H-pyrrolo[3,4-c]pyridine-5(6H)-carboxylate (55 mg, 0.24 mmol) and to this was added 2-methoxyethanol (0.65 mL), and N,N-diisopropylethylamine (0.20 mL, 1.2 mmol); the reaction was heated at 115° C. for 16 hours, cooled, diluted with CH2Cl2 (25 mL) and washed with 1 M NaOH (10 mL). The aqueous layer was extracted with CH2Cl2 (15 mL). The combined organics were dried (MgSO4), filtered, concentrated and chromatographed and eluted with a gradient of 1:0 to 0:1 CH2Cl2:EtOAc to provide the title compound.

後処理

  1. temperaturecooled
  2. washwashed with 1 M NaOH (10 mL)
  3. extractionThe aqueous layer was extracted with CH2Cl2 (15 mL)
  4. dry with materialThe combined organics were dried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customchromatographed
  8. washeluted with a gradient of 1:0 to 0:1 CH2Cl2

出典と根拠

ORDレコード
ord-2a8c6eb47bfd4b0687dbd936dc4b2484
出典データセット
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08735411B2

反応ノート

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