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Toluene → 2-[4-(4,6-Bis-trichloromethyl-s-triazin-2-yl) benzoylmethylene]-3-methylbenzothiazoline

HRID 345193
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HRID 345193 반응식
[CH3:1][C:2]1[S:3][C:4]2[CH:11]=[CH:10][CH:9]=[CH:8][C:5]=2[N+:6]=1[CH3:7].CC1C=CC(S(O)(=O)=O)=CC=1.[Cl:23][C:24]([Cl:45])([Cl:44])[C:25]1[N:30]=[C:29]([C:31]([Cl:34])([Cl:33])[Cl:32])[N:28]=[C:27]([C:35]2[CH:43]=[CH:42][C:38]([C:39](Cl)=[O:40])=[CH:37][CH:36]=2)[N:26]=1.C1(C)C=CC=CC=1>C(N(CC)CC)C>[Cl:34][C:31]([Cl:32])([Cl:33])[C:29]1[N:30]=[C:25]([C:24]([Cl:45])([Cl:23])[Cl:44])[N:26]=[C:27]([C:35]2[CH:36]=[CH:37][C:38]([C:39]([CH:1]=[C:2]3[N:6]([CH3:7])[C:5]4[CH:8]=[CH:9][CH:10]=[CH:11][C:4]=4[S:3]3)=[O:40])=[CH:42][CH:43]=2)[N:28]=1
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참가 물질

5

반응물 3

HCID 1140TolueneHCID 14473251HCID 14473251, 화합물HCID 867451362,3-Dimethyl-benzothiazolium p-toluenesulfonate

생성물 1

HCID 867451372-[4-(4,6-Bis-trichloromethyl-s-triazin-2-yl) benzoylmethylene]-3-methylbenzothiazoline

시약·촉매·용매 1

HCID 8471Triethylamine용매

실험 절차

2,3-Dimethylbenzothiazolium-p-toluenesulfonate (13.4 pbw) and 4-(4,6-bis-trichloromethyl-s-triazin2-yl)-benzoylchloride (22.7 pbw) are successively suspended or dissolved, respectively, in 150 pbw of toluene. The mixture is cooled to 15° C. and with the exclusion of moisture 13.1 pbw of triethylamine are added dropwise at this temperature. The mixture discolors towards dark brown and is stirred for 3 hours at room temperature. The precipitate formed is removed by filtration with suction and washed with cold toluene. The residue is digested in 200 pbw of methanol and stirred for about 60 minutes, again filtered and dried.

후처리

  1. dissolutiondissolved
  2. additionare added dropwise at this temperature
  3. customThe precipitate formed
  4. customis removed by filtration with suction
  5. washwashed with cold toluene
  6. stirringstirred for about 60 minutes
  7. filtrationagain filtered
  8. customdried

출처 및 근거

ORD 기록
ord-c979926e303f4c88b1dbb09f16ae3759
출처 데이터셋
uspto-grants-1991_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05055579

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