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Acetone → HCID 12223714, 화합물

HRID 1658060
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HRID 1658060 반응식
[F:1][C:2]([F:23])([F:22])[C:3]1[CH:16]=[CH:15][C:14]2[S:13][C:12]3[C:7]4=[C:8]([C:17](=[O:21])[NH:18][C:19](=[S:20])[N:6]4[C:5]=2[CH:4]=1)[CH:9]=[CH:10][CH:11]=3.[OH-].[K+].[CH3:26]C(C)=O.CI>O>[CH3:26][S:20][C:19]1[N:6]2[C:7]3[C:12]([S:13][C:14]4[CH:15]=[CH:16][C:3]([C:2]([F:1])([F:22])[F:23])=[CH:4][C:5]=42)=[CH:11][CH:10]=[CH:9][C:8]=3[C:17](=[O:21])[N:18]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 180AcetoneHCID 6328Methyl iodideHCID 14797Potassium HydroxideHCID 12223713HCID 12223713, 화합물

생성물 1

HCID 12223714HCID 12223714, 화합물

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

10-Trifluoromethyl-1H-pyrimido[5,4,3-kl]phenothiazine-3-one-1(2H)-thione (53.6 g., 0.152 mol.) was added to a stirred solution of 8.95 g. (0.160 mol.) of potassium hydroxide in 1680 ml. of acetone and 720 ml. of water. After all the solid had dissolved and a clear yellow solution formed, 22.8 g. (10 ml., 0.160 mol.) of methyl iodide was added in one portion. The reaction mixture was stirred at 25° for 18 hours, diluted with 1000 ml. of water and chilled in an ice-bath for several hours. The resulting light yellow solid was collected by filtration and washed with water to give 1-methylmercapto-10-trifluoromethyl-3H-pyrimido[5,4,3-kl]phenothiazine-3-one, m.p. 229°-231° (ethanol).

후처리

  1. dissolutionAfter all the solid had dissolved
  2. customa clear yellow solution formed
  3. additiondiluted with 1000 ml
  4. filtrationThe resulting light yellow solid was collected by filtration
  5. washwashed with water

출처 및 근거

ORD 기록
ord-4e2b4c933d614fffae55a6cf8bf5b2ad
출처 데이터셋
uspto-grants-1976_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03962438

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