Iodoethane → 10-(1-Diethylamino-2-propyl)-2-phenothiazinecarbonitrile

HRID 704196노트

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HRID 704196 반응식
[CH2:1]([NH:3][CH2:4][CH:5]([N:7]1[C:20]2[CH:19]=[C:18]([C:21]#[N:22])[CH:17]=[CH:16][C:15]=2[S:14][C:13]2[C:8]1=[CH:9][CH:10]=[CH:11][CH:12]=2)[CH3:6])[CH3:2].C(=O)([O-])[O-].[Na+].[Na+].I[CH2:30][CH3:31]>CN(C)C=O>[CH2:1]([N:3]([CH2:30][CH3:31])[CH2:4][CH:5]([N:7]1[C:20]2[CH:19]=[C:18]([C:21]#[N:22])[CH:17]=[CH:16][C:15]=2[S:14][C:13]2[C:8]1=[CH:9][CH:10]=[CH:11][CH:12]=2)[CH3:6])[CH3:2]

참가 물질

5

반응물 3

HCID 6340IodoethaneHCID 10340Sodium CarbonateHCID 14536548HCID 14536548, 화합물

생성물 1

HCID 1453650710-(1-Diethylamino-2-propyl)-2-phenothiazinecarbonitrile

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
150 °C

실험 절차

A mixture of 10-(1-ethylamino-2-propyl)-2-phenothiazinecarbonitrile acid fumarate, D series (4 g), sodium carbonate (1.32 g) and iodoethane (1 cc) in dimethylformamide (50 cc) is heated to a temperature in the region of 150° C. for 6 hours. After cooling, the reaction mixture is concentrated to dryness (30 m Hg; 4 kPa) at 50° C. and the residue is taken up with ethyl acetate (100 cc) and washed successively with distilled water (50 cc) and with saturated aqueous sodium chloride solution (50 cc). The organic phase is dried over magnesium sulphate, filtered and concentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 40° C. 10-(1-diethylamino-2-propyl)-2-phenothiazinecarbonitrile, D series (3.4 g) is thereby obtained in the form of a yellow oil.

후처리

  1. temperatureAfter cooling
  2. concentrationthe reaction mixture is concentrated to dryness (30 m Hg; 4 kPa) at 50° C.
  3. washwashed successively with distilled water (50 cc) and with saturated aqueous sodium chloride solution (50 cc)
  4. dry with materialThe organic phase is dried over magnesium sulphate
  5. filtrationfiltered
  6. concentrationconcentrated to dryness under reduced pressure (30 mm Hg; 4 kPa) at 40° C

출처 및 근거

ORD 기록
ord-e4ea84fe2a034bd0a2478a29e730ca59
출처 데이터셋
uspto-grants-1991_01
특허 번호
US04985419

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