Carbon Tetrachloride → Tert-butyl 4-chloro-6-methyl-5,8-dihydropyrido[3,4-D]pyrimidine-7(6H)-carboxylate

HRID 450234

反応式

HRID 450234 の反応式
[C:1]([O:5][C:6]([N:8]1[CH:17]([CH3:18])[CH2:16][C:15]2[C:14](=O)[NH:13][CH:12]=[N:11][C:10]=2[CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C(Cl)(Cl)(Cl)[Cl:40]>ClCCCl>[C:1]([O:5][C:6]([N:8]1[CH:17]([CH3:18])[CH2:16][C:15]2[C:14]([Cl:40])=[N:13][CH:12]=[N:11][C:10]=2[CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]

参加物

5

反応物 3

HCID 5943Carbon TetrachlorideHCID 11776TriphenylphosphineHCID 136158782tert-Butyl 6-methyl-4-oxo-4,5,6,8-tetrahydropyrido[3,4-d]pyrimidine-7(1H)-carboxylate

生成物 1

HCID 59394353Tert-butyl 4-chloro-6-methyl-5,8-dihydropyrido[3,4-D]pyrimidine-7(6H)-carboxylate

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

実験手順

A solution of (±)-6-methyl-4-oxo-4,5,6,8-tetrahydro-3H-pyrido[3,4-d]pyrimidine-7-carboxylic acid tert-butyl ester, (7.5 g, 28.3 mmol), triphenylphosphine (14.8 g, 56.5 mmol) and carbon tetrachloride (8.2 mL, 85 mmol) in 1,2-DCE (100 mL) is heated at 80° C. for 6 h. At that time the solution is concentrated in vacuo and the residue is separated via FCC (5-60% EtOAc/heptane) to give the title compound. MS (ESI) m/z 284.1 (M+H).

後処理

  1. concentrationAt that time the solution is concentrated in vacuo
  2. customthe residue is separated via FCC (5-60% EtOAc/heptane)

出典と根拠

ORDレコード
ord-7d1da397b7c344d8b5ebb2b31d846876
出典データセット
uspto-grants-2013_07
特許番号
US08486954B2

関連ノート

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