Hydrochloric Acid → Amino-5-phenyl-7-bis (2 cyanoethyl)amino phenazinium chloride

HRID 22466

반응식

HRID 22466 반응식
[C:1]([CH2:3][CH2:4][N:5]([CH2:13][CH2:14][C:15]#[N:16])[C:6]1[CH:12]=[CH:11][C:9]([NH2:10])=[CH:8][CH:7]=1)#[N:2].[NH2:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.[ClH:24].[Cr](O[Cr]([O-])(=O)=O)([O-])(=O)=O.[Na+].[Na+]>O>[Cl-:24].[NH2:17][C:18]1[C:23]2[C:22](=[N+:5]([C:6]3[CH:12]=[CH:11][CH:9]=[CH:8][CH:7]=3)[C:8]3[C:9]([N:10]=2)=[CH:11][CH:12]=[C:6]([N:5]([CH2:4][CH2:3][C:1]#[N:2])[CH2:13][CH2:14][C:15]#[N:16])[CH:7]=3)[CH:21]=[CH:20][CH:19]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric Acid2회HCID 6115AnilineHCID 25408Sodium DichromateHCID 137971604-(Bis-(2-cyanoethyl)amino) aniline

생성물 1

HCID 67782101Amino-5-phenyl-7-bis (2 cyanoethyl)amino phenazinium chloride

시약·촉매·용매 1

HCID 962Water용매5회

반응 조건

온도
0 °C

실험 절차

A 3-liter round-bottomed flask fitted with a mechanical stirrer was loaded with 16.6 g (0.066 mole) of 4-(bis-(2-cyanoethyl)amino) aniline in 800 ml of distilled water. A 10% excess of aniline (13.56 g, 0.1456 mole) and 200 ml of distilled water were added to the mixture. The mixture was cooled to 0° C. in an ice bath, and 10 g concentrated hydrochloric acid in 25 ml of water were added. Then 6.31 g (0.0883 mole) of sodium dichromate in 25 ml of water was added. The temperature rose to 7° C. Stirring was continued as 9 ml of concentrated hydrochloric acid in 25 ml of distilled water was added over a period of two hours. After 16 hours the temperature had risen to 20° C. The mixture was heated under reflux for 4 hours and then filtered hot. The filter cake was washed with 1.5 liters of boiling water. The combined filtrates were concentrated to 1.4 liters and then heated to 75° C. as 200 g of sodium chloride were added.

후처리

  1. customA 3-liter round-bottomed flask fitted with a mechanical stirrer
  2. customrose to 7° C
  3. additionwas added over a period of two hours
  4. temperatureThe mixture was heated
  5. temperatureunder reflux for 4 hours
  6. filtrationfiltered hot
  7. washThe filter cake was washed with 1.5 liters of boiling water
  8. concentrationThe combined filtrates were concentrated to 1.4 liters
  9. temperatureheated to 75° C. as 200 g of sodium chloride
  10. additionwere added

출처 및 근거

ORD 기록
ord-8d66673dbc1d4507802c4490079168b9
출처 데이터셋
uspto-grants-1995_06
특허 번호
US05428161

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