Tetraglyme → HCID 19862111、化合物

HRID 1165537

反応式

HRID 1165537 の反応式
[CH3:1][N:2]([CH2:7][CH:8]([OH:10])[CH3:9])[CH2:3][CH:4](O)[CH3:5].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.COCCOCCOCCOCCOC>O.[Ru](Cl)(Cl)Cl>[CH3:5][CH:4]1[CH2:3][N:2]([CH3:1])[CH:7]=[C:8]([CH3:9])[O:10]1

参加物

5

反応物 3

HCID 8925TetraglymeHCID 11776TriphenylphosphineHCID 956552-Propanol, 1,1'-(methylimino)bis-2 回

生成物 1

HCID 19862111HCID 19862111、化合物収率 65%

試薬・触媒・溶媒 1

HCID 6093376Ruthenium trichloride hydrate触媒

反応条件

温度
180 °C

実験手順

A mixture of N-methyl-bis-(2-hydroxypropyl)amine (75g, 0.51 mol), trans-4-phenyl-3-buten-2-one (75g, 10.51 mol), ruthenium trichloride hydrate (0.626g 12.3 mmole), triphenylphosphine (2.0g 17.6 mmole), and tetraglyme (30g) was added to a 250-ml 3-neck round bottom flask connected with a fractional distillation set and a thermometer. The reaction was heated to 180° C. under nitrogen and the products were distilled out through the distillation set. The products (organic layer) were then fractionally distilled again to obtain a 65% yield of 3,4-dihydro-2,4,6-trimethyl-2H-1,4-oxazine.

後処理

  1. additionwas added to a 250-ml 3-neck round bottom flask
  2. distillationconnected with a fractional distillation
  3. distillationthe products were distilled out through the distillation
  4. distillationThe products (organic layer) were then fractionally distilled again

出典と根拠

ORDレコード
ord-9f0269cca29547f29e294bb170fed892
出典データセット
uspto-grants-1990_03
特許番号
US04910303

関連ノート

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