Hexamethylenetetramine → 2-Amino-1-((1,1'-biphenyl)-4-yl)ethan-1-one hydrochloride

HRID 1073250ノート

反応式

HRID 1073250 の反応式
Br[CH2:2][C:3]([C:5]1[CH:10]=[CH:9][C:8]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=[CH:7][CH:6]=1)=[O:4].C1N2CN3CN(C2)C[N:18]1C3.C(Cl)(Cl)[Cl:28]>>[ClH:28].[NH2:18][CH2:2][C:3]([C:5]1[CH:10]=[CH:9][C:8]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=[CH:7][CH:6]=1)=[O:4]

参加物

4

反応物 3

HCID 4101HexamethylenetetramineHCID 6212ChloroformHCID 672821-(1,1'-Biphenyl)-4-yl-2-bromoethanone

生成物 1

HCID 124871822-Amino-1-((1,1'-biphenyl)-4-yl)ethan-1-one hydrochloride

反応条件

温度
48 °C

実験手順

To 400 ml of chloroform in a 3 liter flask equipped with a mechanical stirrer was added 50 g of 2-bromo-4'-phenylacetophenone and 26.4 g of hexamethylenetetramine. The solution was stirred at 48° C. for 4 hours, then cooled to 20° C., and the resulting solid collected and washed with a small amount of absolute ethanol. The solid was suspended in a solution of 270 ml of absolute ethanol and 134 ml of concentrated hydrochloric acid and stirred at 20° C. for 22 hours. This solid was collected washed with 100 ml of water and dried at 75° C. in vacuo, giving 54.9 g of the desired compound as a white solid, mp 260° C.

後処理

  1. temperaturecooled to 20° C.
  2. customthe resulting solid collected
  3. washwashed with a small amount of absolute ethanol
  4. stirringstirred at 20° C. for 22 hours
  5. customThis solid was collected
  6. washwashed with 100 ml of water
  7. customdried at 75° C. in vacuo

出典と根拠

ORDレコード
ord-1e956132c9014febb9495d4297927714
出典データセット
uspto-grants-1990_11
特許番号
US04968702

反応ノート

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