Water → HCID 178441902, 화합물

HRID 398993노트

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HRID 398993 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 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 reaction medium was poured into 100 ml of ice-cooled water, separated and washed with ice-cooled water. The moist product was taken up in 100 ml of water and alkalized with concentrated ammonium hydroxide. After separation, the residue was washed with water and dried at 70° C. under reduced pressure to obtain 1.47 g of the expected product melting at 180° C.

후처리

  1. waitfor one hour at 100° C
  2. customseparated
  3. washwashed with ice-
  4. temperaturecooled water
  5. customAfter separation
  6. washthe residue was washed with water
  7. customdried at 70° C. under reduced pressure

출처 및 근거

ORD 기록
ord-e38725138e7f4e8fbd8b7be6a58b495d
출처 데이터셋
uspto-grants-1998_10
특허 번호
US05817674

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