Ammonia → 16459-44-2

HRID 459674

반응식

HRID 459674 반응식
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([NH:10][NH2:11])=[CH:6][CH:5]=1)([O-:3])=[O:2].Cl.C[N:14](C)[CH:15]=[CH:16][C:17]#N.N>O.C(O)CC>[NH2:14][C:15]1[N:10]([C:7]2[CH:6]=[CH:5][C:4]([N+:1]([O-:3])=[O:2])=[CH:9][CH:8]=2)[N:11]=[CH:17][CH:16]=1

참가 물질

7

반응물 4

HCID 222AmmoniaHCID 313Hydrochloric AcidHCID 974973-(Dimethylamino)prop-2-enenitrile2회HCID 3310889(4-Nitrophenyl)hydrazine

생성물 1

HCID 1267877116459-44-2

시약·촉매·용매 2

HCID 962Water용매HCID 10311-Propanol용매

실험 절차

7.65 g (50 mmol) of 4-nitrophenylhydrazine was suspended in 70 mL of water and 10 mL of n-propanol and the suspension was heated to about 50° C. At this temperature, 5 g (50 mmol) of concentrated hydrochloric acid and 4.81 g (50 mmol) of 3-dimethylaminoacrylonitrile were then added. After an additional 15 minutes, 3.8 mL (50 mmol) of a 25% ammonia solution was added dropwise within 15 minutes. The reaction mixture was then allowed to agitate at about 50° C. until the 3-dimethylaminoacrylonitrile had completely reacted (about 1 hour) after which the resulting dark-brown suspension was cooled in an ice bath. The precipitate was filtered off, washed 3 times with small portions of cold water and then dried. Yield of crude product: 9.4 g (46 mmol. 92% of the theoretical).

후처리

  1. customhad completely reacted (about 1 hour) after which the resulting dark-brown suspension
  2. temperaturewas cooled in an ice bath
  3. filtrationThe precipitate was filtered off
  4. washwashed 3 times with small portions of cold water
  5. customdried

출처 및 근거

ORD 기록
ord-6bac166120524a40b37f69db9f43e5ef
출처 데이터셋
uspto-grants-2007_03
특허 번호
US07195649B2

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