Water → HCID 178441902、化合物

HRID 1602941ノート

反応式

HRID 1602941 の反応式
[N:1]([O-])=O.[Na+].[C:5]([C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1[NH2:17])#[C:6][CH2:7][CH2:8][CH2:9][CH3:10].[OH2:18]>Cl>[CH2:7]([C:6]1[N:1]=[N:17][C:12]2[C:11]([C:5]=1[OH:18])=[CH:16][CH:15]=[CH:14][CH:13]=2)[CH2:8][CH2:9][CH3:10]

参加物

5

反応物 3

HCID 962Water2 回HCID 107973102-(Hex-1-yn-1-yl)anilineHCID 23668193Sodium Nitrite

生成物 1

HCID 178441902HCID 178441902、化合物

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

反応条件

温度
0 °C

実験手順

A solution of 2 g of sodium nitrite in 60 ml of water was added at 0° C. to a suspension prepared at 0° C. of 3.2 g of the product of Step A in 100 ml of concentrated hydrochloric acid and the mixture was stirred for 90 minutes at 0° C., then for one hour at 100° C. The cooled reaction mixture was poured into 100 ml of ice-cooled water and after separating and washing with water, the moist crude product was taken up in 100 ml of water, alkalinized with concentrated ammonium hydroxide, separated and washed with water to obtain after drying at 70° C., 1.47 g of the desired product melting at 180° C.

後処理

  1. waitfor one hour at 100° C
  2. customThe cooled reaction mixture
  3. customafter separating
  4. washwashing with water
  5. customseparated
  6. washwashed with water
  7. customto obtain
  8. customafter drying at 70° C.

出典と根拠

ORDレコード
ord-a1d2ca665c7a4ea68004f39b87d99457
出典データセット
uspto-grants-1999_11
特許番号
US05985894

反応ノート

読み込み中…