Sodium Hydroxide → 3-Amino-9-ethylcarbazole

HRID 1763218

반응식

HRID 1763218 반응식
[N+:1]([C:4]1[CH:5]=[CH:6][C:7]2[N:8]([CH2:17][CH3:18])[C:9]3[C:14]([C:15]=2[CH:16]=1)=[CH:13][CH:12]=[CH:11][CH:10]=3)([O-])=O.[OH-].[Na+]>Cl.O>[NH2:1][C:4]1[CH:5]=[CH:6][C:7]2[N:8]([CH2:17][CH3:18])[C:9]3[C:14]([C:15]=2[CH:16]=1)=[CH:13][CH:12]=[CH:11][CH:10]=3

참가 물질

5

반응물 2

HCID 14798Sodium HydroxideHCID 665739-ethyl-3-nitro-9H-carbazole

생성물 1

HCID 85883-Amino-9-ethylcarbazole수율 82.8%

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 962Water용매

실험 절차

A solution of 10.2 g of 3-nitro-N-ethylcarbazole (42.5 mmol) and 38.4 g of stannous chloride dihydrate (170 mmol) in 100 ml of concentrated hydrochloric acid was heated for 3 hours at 92° C. The ice cooled solution was (cautiously) made basic by partial addition of a solution of 75 g sodium hydroxide in 150 ml of water. The product was filtered off and washed with the above base solution, followed by copious amounts of water, and then air dried. Vacuum drying and recrystallization from pyridine/water gave 7.4 g light-green needles (82% yield) mp b 109°-11° C.

후처리

  1. filtrationThe product was filtered off
  2. washwashed with the above base solution
  3. customair dried
  4. customVacuum drying
  5. customrecrystallization from pyridine/water

출처 및 근거

ORD 기록
ord-2e9d8db71f794180825067f2db8a5a8d
출처 데이터셋
uspto-grants-1978_09
특허 번호
US04111850

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