HCID 19046449, 화합물 → HCID 19046432, 화합물

HRID 1439936노트

반응식

HRID 1439936 반응식
[C:1]([C:5]1[CH:11]=[C:10]([CH2:12]SC)[C:8]([NH2:9])=[C:7]([Cl:15])[CH:6]=1)([CH3:4])([CH3:3])[CH3:2]>CO.[Ni]>[C:1]([C:5]1[CH:11]=[C:10]([CH3:12])[C:8]([NH2:9])=[C:7]([Cl:15])[CH:6]=1)([CH3:4])([CH3:3])[CH3:2]

참가 물질

4

반응물 1

HCID 19046449HCID 19046449, 화합물

생성물 1

HCID 19046432HCID 19046432, 화합물

시약·촉매·용매 2

HCID 935Nickel촉매HCID 887Methanol용매

실험 절차

4-t-Butyl-2-chloro-6-(methylthiomethyl)aniline (1.3 g) was dissolved in methanol (50 ml) and Raney nickel (prewashed to pH 7) was added portionwise until t.l.c. indicated all starting material had reacted (ether-hexane, 1:10). The Raney nickel was removed by filtration through celite and the flitrate was evaporated. The residue was dissolved in ether and washed with brine, dried (MgSO4) and evaporated. The residue was purified on silica using hexane--5% ether in hexane as eluant to afford the product as a yellow liquid. 1H NMR (360 MHz, CDCl3) δ 1.26 (9H, s; (CH3)3), 2.19 (3H, s, CH3), 3.97 (2H, s, NH2), 6.97 (1H, d, J=2.0 Hz, ArH), 7.14 (1H, d, J=2.0 Hz, ArH).

후처리

  1. customThe Raney nickel was removed by filtration through celite
  2. customthe flitrate was evaporated
  3. dissolutionThe residue was dissolved in ether
  4. washwashed with brine
  5. dry with materialdried (MgSO4)
  6. customevaporated
  7. customThe residue was purified on silica

출처 및 근거

ORD 기록
ord-0cf5db6318194e4a8092e8b906c1509b
출처 데이터셋
uspto-grants-1996_03
특허 번호
US05496833

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