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Methanol → 1,5-Bis(mesitylamino)-3,7-bis(phenylmercapto)-anthraquinone

HRID 1372796
ノート
印刷プレビュー

反応式

HRID 1372796 の反応式
[C:1]1([CH3:38])[CH:6]=[C:5]([CH3:7])[CH:4]=[C:3]([CH3:8])[C:2]=1[NH:9][C:10]1[C:23]2[C:22](=[O:24])[C:21]3[C:16](=[C:17]([NH:26][C:27]4[C:32]([CH3:33])=[CH:31][C:30]([CH3:34])=[CH:29][C:28]=4[CH3:35])[CH:18]=[C:19](Br)[CH:20]=3)[C:15](=[O:36])[C:14]=2[CH:13]=[C:12](Br)[CH:11]=1.[C:39]1([S-:45])[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=1.[Na+].CO>CN(C=O)C>[C:1]1([CH3:38])[CH:6]=[C:5]([CH3:7])[CH:4]=[C:3]([CH3:8])[C:2]=1[NH:9][C:10]1[C:23]2[C:22](=[O:24])[C:21]3[C:16](=[C:17]([NH:26][C:27]4[C:32]([CH3:33])=[CH:31][C:30]([CH3:34])=[CH:29][C:28]=4[CH3:35])[CH:18]=[C:19]([S:45][C:39]4[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=4)[CH:20]=3)[C:15](=[O:36])[C:14]=2[CH:13]=[C:12]([S:45][C:39]2[CH:44]=[CH:43][CH:42]=[CH:41][CH:40]=2)[CH:11]=1
参加物反応条件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 887MethanolHCID 4110039Sodium benzenethiolateHCID 21072034HCID 21072034、化合物

生成物 1

HCID 210720331,5-Bis(mesitylamino)-3,7-bis(phenylmercapto)-anthraquinone

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

反応条件

温度
120 °C

実験手順

16.5 g of 1,5-bis(mesitylamino)-3,7-dibromoanthraquinone are suspended at RT in 50 ml of DMF and heated to 120° C. After cooling to 50° C., a suspension of 8.5 g of sodium thiophenolate in 25 ml of DMF is added thereto. The mixture is then heated to 120° C. again and stirred at that temperature for 1.5 hours. After cooling the mixture to 60° C., 100 ml of methanol are added and the mixture is stirred overnight at RT. The precipitate is filtered off, washed with a methanol/water mixture (1:1) and dried in vacuo.

後処理

  1. temperatureAfter cooling to 50° C.
  2. additionis added
  3. temperatureThe mixture is then heated to 120° C. again
  4. temperatureAfter cooling the mixture to 60° C.
  5. stirringthe mixture is stirred overnight at RT
  6. filtrationThe precipitate is filtered off
  7. washwashed with a methanol/water mixture (1:1)
  8. customdried in vacuo

出典と根拠

ORDレコード
ord-4036e7137c384ab58c6e787b8a9a30f5
出典データセット
uspto-grants-2007_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07160335B2

反応ノート

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