C-(2,3-dihydro-benzo[1,4]dioxin-5-yl)-methyleneamine → 1-(2,3-Dihydro-benzo[1,4]dioxin-5-yl)-ethylamine

HRID 1988419ノート

反応式

HRID 1988419 の反応式
[O:1]1[C:6]2[CH:7]=[CH:8][CH:9]=[C:10]([CH:11]=[NH:12])[C:5]=2[O:4][CH2:3][CH2:2]1.[CH3:13][Mg]Br>C1(C)C=CC=CC=1.C(OCC)C>[O:1]1[C:6]2[CH:7]=[CH:8][CH:9]=[C:10]([CH:11]([NH2:12])[CH3:13])[C:5]=2[O:4][CH2:3][CH2:2]1

参加物

5

反応物 2

HCID 86618567C-(2,3-dihydro-benzo[1,4]dioxin-5-yl)-methyleneamineHCID 178418573HCID 178418573、化合物

生成物 1

HCID 577255011-(2,3-Dihydro-benzo[1,4]dioxin-5-yl)-ethylamine

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 3283Diethyl Ether溶媒

反応条件

温度
60 °C

実験手順

The dried resin to which the C-(2,3-dihydro-benzo[1,4]dioxin-5-yl)-methyleneamine (1 eq) was bound was suspended in dry toluene. Under a nitrogen atmosphere methyl magnesium bromide (150 eq) in a 3 M solution in ethyl ether was added. This mixture was shaken for 24 hours at 60° C. then filtered and washed with toluene, water, then methanol and dichloromethane alternately three times. The final wash was with methanol. The solid was dried under vacuum.

後処理

  1. filtrationthen filtered
  2. washwashed with toluene, water
  3. washThe final wash
  4. customThe solid was dried under vacuum

出典と根拠

ORDレコード
ord-52c249de9ebb4430914271b157d44391
出典データセット
uspto-grants-2009_06
特許番号
US07553854B2

反応ノート

読み込み中…