Phosphorus oxychloride → HCID 59312360、化合物

HRID 2077053ノート

反応式

HRID 2077053 の反応式
P(Cl)(Cl)([Cl:3])=O.[CH2:6]([N:13]1[CH2:19][CH2:18][C:17]2[C:20](=O)[NH:21][C:22]([CH2:24][C:25]3[CH:30]=[CH:29][CH:28]=[C:27]([Cl:31])[CH:26]=3)=[N:23][C:16]=2[CH2:15][CH2:14]1)[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1>[Cl-].C([N+](CC)(CC)CC)C.C(#N)CC>[CH2:6]([N:13]1[CH2:19][CH2:18][C:17]2[C:20]([Cl:3])=[N:21][C:22]([CH2:24][C:25]3[CH:30]=[CH:29][CH:28]=[C:27]([Cl:31])[CH:26]=3)=[N:23][C:16]=2[CH2:15][CH2:14]1)[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1

参加物

5

反応物 2

HCID 24813Phosphorus oxychlorideHCID 136058092HCID 136058092、化合物

生成物 1

HCID 59312360HCID 59312360、化合物収率 87.7%

試薬・触媒・溶媒 2

HCID 5946Tetraethylammonium Chloride触媒HCID 7854Propionitrile溶媒

反応条件

温度
100 °C

実験手順

Phosphoryl chloride (1.33 ml, 14.3 mmol) and tetra-ethyl ammonium chloride (472 mg, 2.85 mmol) were added to a solution of the product of Step A (361 mg, 0.95 mmol) in propionitrile (10 ml) and heated to 100° C. for 17 h. The reaction mixture was concentrated in vacuo then azeotroped with toluene then dichloromethane. The residue was partitioned between dichloromethane (30 ml) and water (20 ml), stirred for 30 min then the organic layer was separated, dried over magnesium sulphate and concentrated in vacuo to give the title compound as a foam in 87.7% yield, 332 mg.

後処理

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. customthen azeotroped with toluene
  3. customThe residue was partitioned between dichloromethane (30 ml) and water (20 ml)
  4. customthe organic layer was separated
  5. dry with materialdried over magnesium sulphate
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-e199dbeaa8ed49efb3200f3aec78b74f
出典データセット
uspto-grants-2011_04
特許番号
US07928099B2

反応ノート

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