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Morpholine → N-[4-(5H-pyrrolo-[2,1-c][1,4]benzodiazepin10(11H)-ylcarbonyl)phenyl]4-morpholineacetamide

HRID 3597
ノート
印刷プレビュー

反応式

HRID 3597 の反応式
Cl[CH2:2][C:3]([NH:5][C:6]1[CH:11]=[CH:10][C:9]([C:12]([N:14]2[C:20]3[CH:21]=[CH:22][CH:23]=[CH:24][C:19]=3[CH2:18][N:17]3[CH:25]=[CH:26][CH:27]=[C:16]3[CH2:15]2)=[O:13])=[CH:8][CH:7]=1)=[O:4].[NH:28]1[CH2:33][CH2:32][O:31][CH2:30][CH2:29]1.CN1CCCN(C)C1=O>C(Cl)Cl>[CH:27]1[CH:26]=[CH:25][N:17]2[CH2:18][C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=3[N:14]([C:12]([C:9]3[CH:10]=[CH:11][C:6]([NH:5][C:3](=[O:4])[CH2:2][N:28]4[CH2:33][CH2:32][O:31][CH2:30][CH2:29]4)=[CH:7][CH:8]=3)=[O:13])[CH2:15][C:16]=12
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8083MorpholineHCID 816462(1H)-Pyrimidinone, tetrahydro-1,3-dimethyl-HCID 218370752-chloro-N-[4-(5H-pyrrolo[2,1-c][1,4]benzodiazepin-10(11H)ylcarbonyl)phenyl]acetamide

生成物 1

HCID 70059534N-[4-(5H-pyrrolo-[2,1-c][1,4]benzodiazepin10(11H)-ylcarbonyl)phenyl]4-morpholineacetamide収率 106.8%

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒

実験手順

A stirred suspension of 0.19 g of 2-chloro-N-[4-(5H-pyrrolo[2,1-c][1,4]benzodiazepin-10(11H)-ylcarbonyl)phenyl]acetamide in 1 ml of methylene chloride is added 0.44 g of morpholine followed by 1 ml of 1,3-di-methyl-3,4,5,6-tetrahydro-2(1H)-pyrimidinone and stirring continued for 20 hours. The methylene chloride is evaporated and the residue diluted with water. The resulting suspension is filtered and the precipitate washed with water. The brown solid is dissolved in 15 ml of ethyl acetate and washed with saturated NaHCO3, brine and dried with Na2SO4. The mixture is filtered and the filtrate evaporated in vacuo to give 0.23 g of a colorless gum which is stirred with ethyl acetate-hexanes to give 0.21 g of white solid. MS(CI): 431(M+H).

後処理

  1. customThe methylene chloride is evaporated
  2. additionthe residue diluted with water
  3. filtrationThe resulting suspension is filtered
  4. washthe precipitate washed with water
  5. dissolutionThe brown solid is dissolved in 15 ml of ethyl acetate
  6. washwashed with saturated NaHCO3, brine
  7. dry with materialdried with Na2SO4
  8. filtrationThe mixture is filtered
  9. customthe filtrate evaporated in vacuo

出典と根拠

ORDレコード
ord-b58a69d7ccb643e6b7543dcded01e2ce
出典データセット
uspto-grants-1998_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05733905

反応ノート

読み込み中…

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