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Iodoethane → HCID 12223716, 화합물

HRID 1658062
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HRID 1658062 반응식
[H-].[Na+].[F:3][C:4]([F:25])([F:24])[C:5]1[CH:18]=[CH:17][C:16]2[S:15][C:14]3[C:9]4=[C:10]([C:19](=[O:23])[NH:20][C:21](=[O:22])[N:8]4[C:7]=2[CH:6]=1)[CH:11]=[CH:12][CH:13]=3.[CH2:26](I)[CH3:27]>CN(C)C=O>[CH2:26]([N:20]1[C:19](=[O:23])[C:10]2[CH:11]=[CH:12][CH:13]=[C:14]3[S:15][C:16]4[CH:17]=[CH:18][C:5]([C:4]([F:24])([F:3])[F:25])=[CH:6][C:7]=4[N:8]([C:9]=23)[C:21]1=[O:22])[CH3:27]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6340IodoethaneHCID 24758Sodium hydrideHCID 1222371510-Trifluoromethyl-1H-pyrimido[5,4,3-kl]phenothiazine-1,3-(2H)-dione

생성물 1

HCID 12223716HCID 12223716, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

57% Sodium hydride in mineral oil (4.2 g., 0.100 mol.) was added to a stirred solution of 28.0 g. (0.0834 mol.) of 10-trifluoromethyl-1H-pyrimido[5,4,3-kl]phenothiazine -1,3(2H)-dione in 220 ml. of dry dimethylformamide. The mixture was stirred for 1 hour at 25°, then 16.8 g. (8.6 ml., 0.108 mol.) of ethyl iodide was added. The resulting greenish yellow, turbid mixture was stirred for 4.5 hours at 25°, then filtered to give a clear yellow solution. The filtrate was evaporated to dryness under reduced pressure and the residue was triturated with petroleum ether to remove the mineral oil. The crude solid product was precipitated from a methanol-water mixture to give the title compound, m.p. 150°-152° (ethanol).

후처리

  1. stirringThe resulting greenish yellow, turbid mixture was stirred for 4.5 hours at 25°
  2. filtrationfiltered
  3. customto give a clear yellow solution
  4. customThe filtrate was evaporated to dryness under reduced pressure
  5. customthe residue was triturated with petroleum ether
  6. customto remove the mineral oil
  7. customThe crude solid product was precipitated from a methanol-water mixture

출처 및 근거

ORD 기록
ord-4f4a0ce4a33547c2b1a2ea10f675a0d3
출처 데이터셋
uspto-grants-1976_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03962438

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