ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Methanol → HCID 53703941、化合物

HRID 1701160
ノート
印刷プレビュー

反応式

HRID 1701160 の反応式
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[CH:13]=[CH:12][C:11]([CH:14]([S:16]([CH2:18][C:19]([OH:21])=[O:20])=[O:17])[CH3:15])=[CH:10][CH:9]=1.CO.[CH:24]1(N=C=NC2CCCCC2)CCCCC1>C1C=CC=CC=1>[CH3:24][O:20][C:19](=[O:21])[CH2:18][S:16]([CH:14]([C:11]1[CH:12]=[CH:13][C:8]([C:3]2[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=2[F:1])=[CH:9][CH:10]=1)[CH3:15])=[O:17]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 887MethanolHCID 10868DicyclohexylcarbodiimideHCID 20348737HCID 20348737、化合物

生成物 1

HCID 53703941HCID 53703941、化合物

試薬・触媒・溶媒 1

HCID 241Benzene溶媒2 回

実験手順

800 gm (2.61 mol) of the difficultly soluble diastereoisomer of [1-(2'-fluoro-4-biphenylyl)-ethylsulfinyl]-acetic acid, m.p. 164°-165° C., were suspended in 4 liters of benzene and 125.5 gm (3.92 mol) of methanol, and a solution of 648 gm (3.14 mol) of dicyclohexyl-carbodiimide in 650 ml of benzene was added while stirring and cooling at 20°-25° C. The acid dissolved, and dicyclohexylurea precipitated out. The mixture was allowed to stand overnight at room temperature, then the excess of carbodiimide was decomposed by addition of glacial acetic acid, and then 2 liters of water were added, the dicyclohexylurea was suction-filtered off, the organic phase was separated from the filtrate and evaporated in vacuo after drying. The obtained oil (969 gm) was recrystallized from 2.9 liters of isopropanol. Yield: 736 gm (88% of theory); m.p. 75°-77° C.

後処理

  1. temperaturecooling at 20°-25° C
  2. dissolutionThe acid dissolved
  3. customdicyclohexylurea precipitated out
  4. additionthe excess of carbodiimide was decomposed by addition of glacial acetic acid
  5. addition2 liters of water were added
  6. filtrationthe dicyclohexylurea was suction-filtered off
  7. customthe organic phase was separated from the filtrate
  8. customevaporated in vacuo
  9. customafter drying
  10. customThe obtained oil (969 gm) was recrystallized from 2.9 liters of isopropanol

出典と根拠

ORDレコード
ord-e4be456d88074e8289827e72fede01a5
出典データセット
uspto-grants-1980_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04191776

反応ノート

読み込み中…

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