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

HRID 751022노트

반응식

HRID 751022 반응식
[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

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 345198Adams' catalyst촉매HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-cbb4e91f03ef419aacfae46c265e3f5f
출처 데이터셋
uspto-grants-2008_07
특허 번호
US07405235B2

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