Lawesson's reagent → HCID 86641534、化合物

HRID 237335ノート

反応式

HRID 237335 の反応式
[C:1]([O:5][C:6]([N:8]1[CH2:14][C:13]2[CH:15]=[C:16]([Cl:19])[CH:17]=[CH:18][C:12]=2[NH:11][C:10](=O)[CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].COC1C=CC(P2(=S)SP(=S)(C3C=CC(OC)=CC=3)[S:30]2)=CC=1>O1CCCC1>[C:1]([O:5][C:6]([N:8]1[CH2:14][C:13]2[CH:15]=[C:16]([Cl:19])[CH:17]=[CH:18][C:12]=2[NH:11][C:10](=[S:30])[CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]

参加物

4

反応物 2

HCID 87949Lawesson's reagentHCID 67377785tert-Butyl 7-chloro-2-oxo-1,2,3,5-tetrahydro-4H-1,4-benzodiazepine-4-carboxylate

生成物 1

HCID 86641534HCID 86641534、化合物収率 157.1%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of 7-chloro-2-oxo-1,2,3,5-tetrahydro-benzo[1,4]diazepine-4-carboxylic acid tert-butyl ester (41.1 g, 0.139 mol) and 2,4-bis-(4-methoxyphenyl)-1,3,2,4-dithiadiphosphetane-2,4-disulfide (31.5 g, 0.0763 mol) in tetrahydrofuran (1100 ml) was heated at reflux for 3 h. The solvent was evaporated and the residue was triturated in tort-butyl methyl ether. The precipitate was removed by filtration and the filtrate was concentrated to dryness. The residue was crystallized from hot ethanol to give the title compound (37.5 g, 86.4%) as light yellow solid. MS m/e: 311 (M−H+).

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 3 h
  3. customThe solvent was evaporated
  4. customthe residue was triturated in tort-butyl methyl ether
  5. customThe precipitate was removed by filtration
  6. concentrationthe filtrate was concentrated to dryness
  7. customThe residue was crystallized from hot ethanol

出典と根拠

ORDレコード
ord-ba2a3689e207451e884815fbebf5d9b0
出典データセット
uspto-grants-2014_02
特許番号
US08642590B2

反応ノート

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