4-Iodo-3-aminothioanisole → 4-Methylsulfanyl-2'-amino-biphenyl-2-ylamine

HRID 751022ノート

反応式

HRID 751022 の反応式
[CH3:1][S:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[N+:15]([O-])=O)=[C:5]([NH2:18])[CH:4]=1.IC1C=CC(SC)=CC=1N>O=[Pt]=O.C(O)C>[CH3:1][S:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=2[NH2:15])=[C:5]([NH2:18])[CH:4]=1

参加物

5

反応物 2

HCID 597545314-Iodo-3-aminothioanisoleHCID 674031774-Methylsulfanyl-2'-nitro-biphenyl-2-ylamine

生成物 1

HCID 674031524-Methylsulfanyl-2'-amino-biphenyl-2-ylamine

試薬・触媒・溶媒 2

HCID 345198Adams' catalyst触媒HCID 702Ethanol溶媒

実験手順

A flask was charged with ca. 1 mmol of 4-Methylsulfanyl-2′-nitro-biphenyl-2-ylamine, 15 mL of ethanol, and 0.1 mmol of PtO2, and stirred under hydrogen atmosphere at 40 psi for 10 minutes. The reaction mixture was filtered through diatomaceous earth, washed with ethanol, and the combined organic layer was evaporated to dryness. The crude material was purified by preparative HPLC. The same material can also be prepared by the previous method, (Suzuki coupling conditions) starting from 4-iodo-3-aminothioanisole, and purified by preparative HPLC.

後処理

  1. filtrationThe reaction mixture was filtered through diatomaceous earth
  2. washwashed with ethanol
  3. customthe combined organic layer was evaporated to dryness
  4. customThe crude material was purified by preparative HPLC
  5. customThe same material can also be prepared by the previous method, (Suzuki coupling conditions)
  6. custompurified by preparative HPLC

出典と根拠

ORDレコード
ord-cbb4e91f03ef419aacfae46c265e3f5f
出典データセット
uspto-grants-2008_07
特許番号
US07405235B2

反応ノート

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