Propionyl chloride → HCID 178460088、化合物

HRID 2236856ノート

反応式

HRID 2236856 の反応式
[NH2:1][C:2]1[C:3]([OH:24])=[CH:4][C:5]([CH2:8][NH:9][CH:10]=[C:11]2[C:20]3[C:15](=[CH:16][CH:17]=[C:18]([I:21])[CH:19]=3)[C:14](=[O:22])[NH:13][C:12]2=[O:23])=[N:6][CH:7]=1.[C:25](Cl)(=[O:28])[CH2:26][CH3:27]>CC(N(C)C)=O>[OH:24][C:3]1[CH:4]=[C:5]([CH2:8][NH:9][CH:10]=[C:11]2[C:20]3[C:15](=[CH:16][CH:17]=[C:18]([I:21])[CH:19]=3)[C:14](=[O:22])[NH:13][C:12]2=[O:23])[N:6]=[CH:7][C:2]=1[NH:1][C:25](=[O:28])[CH2:26][CH3:27]

参加物

4

反応物 2

HCID 62324Propionyl chlorideHCID 1785080254-[[(5-amino-4-oxo-1H-pyridin-2-yl)methylamino]methylidene]-6-iodoisoquinoline-1,3-dione

生成物 1

HCID 178460088HCID 178460088、化合物

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒

実験手順

A mixture of 4-{[(5-Amino-4-hydroxy-pyridin-2-ylmethyl)-amino]-methylene}-6-iodo-4H-isoquinoline-1,3-dione (332 mg, 0.761 mmole), 6 mL of dimethylacetamide is stirred, then propionyl chloride (705 mg, 7.61 mmole) is added and the reaction mixture stirred for one hour. The reaction mixture is evaporated to dryness, and then stirred overnight with a saturated aqueous sodium bicarbonate solution, the solid is filtered, washed well with water and dried to give a yellow solid, 46 mg, (11%); m.p. 210-18° C. dec; MS (ES+): m/z 492.9 (M+H).

後処理

  1. stirringthe reaction mixture stirred for one hour
  2. customThe reaction mixture is evaporated to dryness
  3. stirringstirred overnight with a saturated aqueous sodium bicarbonate solution
  4. filtrationthe solid is filtered
  5. washwashed well with water
  6. customdried
  7. customto give a yellow solid, 46 mg, (11%)

出典と根拠

ORDレコード
ord-68889b8e50f54cb28af423edaacf326c
出典データセット
uspto-grants-2010_05
特許番号
US07713994B2

反応ノート

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