Dichloromethane → (4-fluorotetrahydro-2H-pyran-4-yl)methanamine

HRID 1035932ノート

反応式

HRID 1035932 の反応式
[F:1][C:2]1([CH2:8][N:9]2C(=O)C3C(=CC=CC=3)C2=O)[CH2:7][CH2:6][O:5][CH2:4][CH2:3]1.NN.C(Cl)Cl>C(O)C>[F:1][C:2]1([CH2:8][NH2:9])[CH2:7][CH2:6][O:5][CH2:4][CH2:3]1

参加物

5

反応物 3

HCID 6344DichloromethaneHCID 9321HydrazineHCID 671270062-((4-Fluorotetrahydro-2h-pyran-4-yl)methyl)isoindoline-1,3-dione

生成物 1

HCID 46856407(4-fluorotetrahydro-2H-pyran-4-yl)methanamine

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of EXAMPLE 138B (1.4 g) and hydrazine (1.548 mL) in ethanol (40 mL) was heated at 70° C. overnight, cooled to room temperature, slurried with CH2Cl2 (200 mL) and the solid removed by filtration. The filtrate was concentrated and chromatographed on silica gel eluting with 100:5:1 ethyl acetate/methanol/NH4OH to give the product.

後処理

  1. customthe solid removed by filtration
  2. concentrationThe filtrate was concentrated
  3. customchromatographed on silica gel eluting with 100:5:1 ethyl acetate/methanol/NH4OH
  4. customto give the product

出典と根拠

ORDレコード
ord-c07a3e95171f48bd8ca3c4d8ad5a4de3
出典データセット
uspto-grants-2013_10
特許番号
US08546399B2

反応ノート

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