Water → HCID 178441902, 화합물

HRID 1602941노트

반응식

HRID 1602941 반응식
[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]

참가 물질

5

반응물 3

HCID 962Water2회HCID 107973102-(Hex-1-yn-1-yl)anilineHCID 23668193Sodium Nitrite

생성물 1

HCID 178441902HCID 178441902, 화합물

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

반응 조건

온도
0 °C

실험 절차

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.

후처리

  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.

출처 및 근거

ORD 기록
ord-a1d2ca665c7a4ea68004f39b87d99457
출처 데이터셋
uspto-grants-1999_11
특허 번호
US05985894

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