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Methanol → 4-(2,4-Dioxo-8-methyl-1,3,8-triazaspiro[4.5]-decan-3-yl)-2-(trifluoromethyl)-benzonitrile

HRID 264021
ノート
印刷プレビュー

反応式

HRID 264021 の反応式
N=[C:2]1[C:6]2([CH2:11][CH2:10][N:9]([CH3:12])[CH2:8][CH2:7]2)[NH:5][C:4](=[O:13])[N:3]1[C:14]1[CH:21]=[CH:20][C:17]([C:18]#[N:19])=[C:16]([C:22]([F:25])([F:24])[F:23])[CH:15]=1.C[OH:27].[OH-].[NH4+].[Cl-].[Na+]>C(OCC)(=O)C>[O:13]=[C:4]1[N:3]([C:14]2[CH:21]=[CH:20][C:17]([C:18]#[N:19])=[C:16]([C:22]([F:25])([F:24])[F:23])[CH:15]=2)[C:2](=[O:27])[C:6]2([CH2:11][CH2:10][N:9]([CH3:12])[CH2:8][CH2:7]2)[NH:5]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 887MethanolHCID 5234Sodium ChlorideHCID 14923Ammonium HydroxideHCID 21846478HCID 21846478、化合物

生成物 1

HCID 218464874-(2,4-Dioxo-8-methyl-1,3,8-triazaspiro[4.5]-decan-3-yl)-2-(trifluoromethyl)-benzonitrile

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate
溶媒

実験手順

Using the procedure of Example 2, 3 g of the product of Example 22, 70 ml of methanol and 17 ml of 2N hydrochloric were reacted and the solution was refluxed for 90 minutes. It was poured into 200 ml of ammonium hydroxide +100 g of ice saturated with sodium chloride and extraction was carried out 4 times with ethyl acetate. The extracts were washed with salt water, dried and purified on silica with methylene chloride-methanol: 9-1 as eluant. After crystallization from methylene chloride-isopropyl ether, 2.12 g of the expected product (white crystals) melting at 188°-189° C were obtained.

後処理

  1. customhydrochloric were reacted
  2. temperaturethe solution was refluxed for 90 minutes
  3. washThe extracts were washed with salt water
  4. customdried
  5. custompurified on silica with methylene chloride-methanol
  6. customAfter crystallization from methylene chloride-isopropyl ether

出典と根拠

ORDレコード
ord-d44bbc50282a497da1673d545a076bb2
出典データセット
uspto-grants-1997_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05646172

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート