Toluene → HCID 86745139、化合物

HRID 345195

反応式

HRID 345195 の反応式
[Cl:1][C:2]([Cl:23])([Cl:22])[C:3]1[N:8]=[C:7]([C:9]([Cl:12])([Cl:11])[Cl:10])[N:6]=[C:5]([C:13]2[CH:21]=[CH:20][C:16]([C:17](Cl)=[O:18])=[CH:15][CH:14]=2)[N:4]=1.[CH3:24][N:25]1[C:33]2[C:28](=[CH:29][CH:30]=[CH:31][CH:32]=2)[C:27]([CH3:35])([CH3:34])[C:26]1=[CH2:36].C(N(CC)CC)C.C1(C)C=CC=CC=1>CCOCC.O>[Cl:11][C:9]([Cl:12])([Cl:10])[C:7]1[N:8]=[C:3]([C:2]([Cl:1])([Cl:22])[Cl:23])[N:4]=[C:5]([C:13]2[CH:21]=[CH:20][C:16]([C:17]([CH:36]=[C:26]3[C:27]([CH3:34])([CH3:35])[C:28]4[C:33](=[CH:32][CH:31]=[CH:30][CH:29]=4)[N:25]3[CH3:24])=[O:18])=[CH:15][CH:14]=2)[N:6]=1

参加物

7

反応物 4

HCID 1140TolueneHCID 83511,3,3-Trimethyl-2-methyleneindolineHCID 8471TriethylamineHCID 14473251HCID 14473251、化合物

生成物 1

HCID 86745139HCID 86745139、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 3283Diethyl Ether溶媒

実験手順

4-(4,6-Bis-trichloromethyl-s-triazin-2-yl)benzoylchloride (15.4 pbw) are added dropwise with stirring at 10° C. to 5.2 pbw of 1,3,3-trimethyl-2-methylene-indoline and 10.6 pbw of triethylamine in 140 pbw of anhydrous toluene. The mixture is stirred for 3 hours at room temperature. It is then admixed with 100 pbw of water and 200 pbw of ether and extracted by shaking. The dried organic phase is concentrated. The residue is recrystallized from 2-methoxy-ethanol, giving red-orange crystals.

後処理

  1. extractionextracted
  2. stirringby shaking
  3. concentrationThe dried organic phase is concentrated
  4. customThe residue is recrystallized from 2-methoxy-ethanol
  5. customgiving red-orange crystals

出典と根拠

ORDレコード
ord-0e364f3de92147eebb472fe12c1927e9
出典データセット
uspto-grants-1991_10
特許番号
US05055579

関連ノート

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