Methylamine → (1-Amino-1H-pyrrol-2-yl)-2-thienylmethanone

HRID 1901282노트

반응식

HRID 1901282 반응식
[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[C:6]([C:8]1[N:9]([N:13]2C(=O)C3C(=CC=CC=3)C2=O)[CH:10]=[CH:11][CH:12]=1)=[O:7].CN>CN(C)C=O.O>[NH2:13][N:9]1[CH:10]=[CH:11][CH:12]=[C:8]1[C:6]([C:2]1[S:1][CH:5]=[CH:4][CH:3]=1)=[O:7]

참가 물질

5

반응물 2

HCID 6329MethylamineHCID 199731582-[2-(2-thienylcarbonyl)-1H-pyrrol-1-yl]-1H-isoindole-1,3(2H)dione

생성물 1

HCID 19973146(1-Amino-1H-pyrrol-2-yl)-2-thienylmethanone수율 64.8%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

To a solution of 2-[2-(2-thienylcarbonyl)-1H-pyrrol-1-yl]-1H-isoindole-1, 3(2H)dione (15.43 g) in 50 ml of dimethylformamide was added 50 ml of 40% methylamine. The reaction mixture was stirred for 1.5 hours at room temperature, diluted with water and extracted with DCM. The combined organic layers were washed with water, dried over magnesium sulfate and evaporated in vacuo. The residual oil was recrystallized from ethyl ether/hexane to afford the product (5.96 g), m.p. 81°-82° C.

후처리

  1. extractionextracted with DCM
  2. washThe combined organic layers were washed with water
  3. dry with materialdried over magnesium sulfate
  4. customevaporated in vacuo
  5. customThe residual oil was recrystallized from ethyl ether/hexane

출처 및 근거

ORD 기록
ord-7fc9c92da1a3476f9fb20961a3c30885
출처 데이터셋
uspto-grants-1996_11
특허 번호
US05576446

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