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

HRID 345193
ノート
印刷プレビュー

反応式

HRID 345193 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 1140TolueneHCID 14473251HCID 14473251、化合物HCID 867451362,3-Dimethyl-benzothiazolium p-toluenesulfonate

生成物 1

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

試薬・触媒・溶媒 1

HCID 8471Triethylamine溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c979926e303f4c88b1dbb09f16ae3759
出典データセット
uspto-grants-1991_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05055579

反応ノート

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