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

HRID 22397

反応式

HRID 22397 の反応式
[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]

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8334f9c353e548a08181c73c94877183
出典データセット
uspto-grants-1995_06
特許番号
US05428053

関連ノート

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