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Methyl 5-methanesulfonyl-4-(4-nitro-3-pentafluorosulfanylphenoxy)-2-methylbenzoate → Methyl 4-(4-amino-3-pentafluorosulfanylphenoxy)-5-methanesulfonyl-2-methylbenzoate

HRID 269418
ノート
印刷プレビュー

反応式

HRID 269418 の反応式
[CH3:1][S:2]([C:5]1[C:6]([O:16][C:17]2[CH:22]=[CH:21][C:20]([N+:23]([O-])=O)=[C:19]([S:26]([F:31])([F:30])([F:29])([F:28])[F:27])[CH:18]=2)=[CH:7][C:8]([CH3:15])=[C:9]([CH:14]=1)[C:10]([O:12][CH3:13])=[O:11])(=[O:4])=[O:3].[H][H]>CC(O)=O.CO.[Pd]>[NH2:23][C:20]1[CH:21]=[CH:22][C:17]([O:16][C:6]2[C:5]([S:2]([CH3:1])(=[O:3])=[O:4])=[CH:14][C:9]([C:10]([O:12][CH3:13])=[O:11])=[C:8]([CH3:15])[CH:7]=2)=[CH:18][C:19]=1[S:26]([F:30])([F:31])([F:27])([F:28])[F:29]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 2

HCID 11648857Methyl 5-methanesulfonyl-4-(4-nitro-3-pentafluorosulfanylphenoxy)-2-methylbenzoateHCID 178418361HCID 178418361、化合物2 回

生成物 1

HCID 59832568Methyl 4-(4-amino-3-pentafluorosulfanylphenoxy)-5-methanesulfonyl-2-methylbenzoate収率 95.3%

試薬・触媒・溶媒 3

HCID 23938Palladium触媒2 回HCID 176
Acetic Acid
溶媒
2 回
HCID 887Methanol溶媒2 回

実験手順

3.80 g of methyl 5-methanesulfonyl-4-(4-nitro-3-pentafluorosulfanylphenoxy)-2-methyl-benzoate were dissolved in 30 ml of HOAc and 30 ml of MeOH, 200 mg of Pd/C (10%) were added, and hydrogenation was carried out under a pressure of 6 bar of hydrogen for 24 h. Since reaction was still incomplete, a further 300 mg of Pd/C (10%), 30 ml of HOAc and 30 ml of MeOH was added, and hydrogenation was continued under a pressure of 6 bar of hydrogen for 24 h. The catalyst was then filtered off and the solvents were removed in vacuo. 3.4 g of a pale gray solid were obtained, mp 175° C. (with decomposition).

後処理

  1. customSince reaction
  2. filtrationThe catalyst was then filtered off
  3. customthe solvents were removed in vacuo

出典と根拠

ORDレコード
ord-eb6e6cde35fb41b3a2b3a0c3370f64d0
出典データセット
uspto-grants-2008_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07446225B2

反応ノート

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