Water → Milveterol

HRID 226285ノート

反応式

HRID 226285 の反応式
[OH:1][C@H:2]([C:27]1[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=1)[CH2:3][NH:4][C:5]1[CH:10]=[CH:9][C:8]([CH2:11][CH2:12][NH:13][CH2:14][C@H:15]([OH:26])[C:16]2[CH:21]=[CH:20][C:19]([OH:22])=[C:18]([NH:23][CH:24]=[O:25])[CH:17]=2)=[CH:7][CH:6]=1.[Cl-:33].[NH4+].O>C(O)(C)C>[ClH:33].[OH:1][C@H:2]([C:27]1[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=1)[CH2:3][NH:4][C:5]1[CH:10]=[CH:9][C:8]([CH2:11][CH2:12][NH:13][CH2:14][C@H:15]([OH:26])[C:16]2[CH:21]=[CH:20][C:19]([OH:22])=[C:18]([NH:23][CH:24]=[O:25])[CH:17]=2)=[CH:7][CH:6]=1.[OH:1][C@H:2]([C:27]1[CH:28]=[CH:29][CH:30]=[CH:31][CH:32]=1)[CH2:3][NH:4][C:5]1[CH:10]=[CH:9][C:8]([CH2:11][CH2:12][NH:13][CH2:14][C@H:15]([OH:26])[C:16]2[CH:21]=[CH:20][C:19]([OH:22])=[C:18]([NH:23][CH:24]=[O:25])[CH:17]=2)=[CH:7][CH:6]=1

参加物

6

反応物 3

HCID 962WaterHCID 25517Ammonium ChlorideHCID 9892481Milveterol

生成物 2

HCID 9892481Milveterol収率 12%HCID 11225217Milveterol hydrochloride

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

In a 200 mL roundbottom flask, compound 1 (200 mg, 0.46 mmol) was dissolved in 40 mL isopropyl alcohol. The solution was stirred and vortexed at room temperature until it became homogeneous. A 7% (w/w) solution of ammonium chloride in water (20 mL, 26 mmol)) was then added dropwise to the stirring solution. The stirring was stopped and the solution was permitted to stand at room temperature for 20 h. White crystals formed. The crystals were collected on a Büchner funnel, washed with 1:1 isopropanol:water (3 mL), and dried for 30 minutes. The crystals were collected to yield the monohydrochloride salt of compound 1 (27 mg, 12% yield).

後処理

  1. customvortexed at room temperature until it
  2. customWhite crystals formed
  3. customThe crystals were collected on a Büchner funnel
  4. washwashed with 1:1 isopropanol
  5. dry with materialwater (3 mL), and dried for 30 minutes
  6. customThe crystals were collected

出典と根拠

ORDレコード
ord-4d7b8181faee4ba8b053ec80d3779f78
出典データセット
uspto-grants-2009_07
特許番号
US07557247B2

反応ノート

読み込み中…