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

HRID 73676ノート

反応式

HRID 73676 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-d984b3b423f440aeb1181f2f44658f6e
出典データセット
uspto-grants-2014_09
特許番号
US08829185B2

反応ノート

読み込み中…