Dimethylformamide → [4-Amino-7-(morpholin-4-ylmethyl)pyrrolo[2,1-f][1,2,4]triazin-6-yl]methanol

HRID 1094870ノート

反応式

HRID 1094870 の反応式
CN(C=O)C.[NH2:6][C:7]1[C:12]2=[CH:13][C:14]([CH2:16][OH:17])=[CH:15][N:11]2[N:10]=[CH:9][N:8]=1.[Cl-].[CH2:19]=[N+:20]1[CH2:25][CH2:24][O:23][CH2:22][CH2:21]1>CO>[NH2:6][C:7]1[C:12]2=[CH:13][C:14]([CH2:16][OH:17])=[C:15]([CH2:19][N:20]3[CH2:25][CH2:24][O:23][CH2:22][CH2:21]3)[N:11]2[N:10]=[CH:9][N:8]=1

参加物

5

反応物 3

HCID 6228DimethylformamideHCID 11367014Morpholinium, 4-methylene-, chlorideHCID 55297730HCID 55297730、化合物

生成物 1

HCID 57955268[4-Amino-7-(morpholin-4-ylmethyl)pyrrolo[2,1-f][1,2,4]triazin-6-yl]methanol収率 90%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of DMF (50 mL) was added (4-aminopyrrolo[2,1-f][1,2,4]triazin-6-yl)methanol (550 mg, 3.35 mmol) and 4-methylenemorpholin-4-ium chloride (Eur. J. Med. Chem. 1989, 24, 379-384) (636 mg, 4.69 mmol). The solution was stirred at rt for 1 h and then the solvent was evaporated. The oil was triturated with CH2Cl2 and a white solid was collected. The free based was obtained by stirring over a Dowex 66 solid support resin in MeOH. The material was filtered and evaporated yielding 794 mg (90%) of the desired product as a white solid. MS [M+H]+=264; LCMS RT=1.07.

後処理

  1. customthe solvent was evaporated
  2. customThe oil was triturated with CH2Cl2
  3. customa white solid was collected
  4. customThe free based was obtained
  5. filtrationThe material was filtered
  6. customevaporated

出典と根拠

ORDレコード
ord-1ead5a46c03c4f77a6b39716e38b698d
出典データセット
uspto-grants-2012_03
特許番号
US08133995B2

反応ノート

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