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Benzene, (triethoxymethyl)- → 1-Acetyl-3-(1-ethoxy-1-phenylmethylidene)-5,6-dimethoxy-2-indolinone

HRID 1007382
ノート
印刷プレビュー

反応式

HRID 1007382 の反応式
[C:1]([N:4]1[C:12]2[C:7](=[CH:8][C:9]([O:15][CH3:16])=[C:10]([O:13][CH3:14])[CH:11]=2)[CH2:6][C:5]1=[O:17])(=[O:3])[CH3:2].[CH3:18][CH2:19][O:20][C:21](OCC)(OCC)[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1>C(OC(=O)C)(=O)C>[C:1]([N:4]1[C:12]2[C:7](=[CH:8][C:9]([O:15][CH3:16])=[C:10]([O:13][CH3:14])[CH:11]=2)[C:6](=[C:21]([O:20][CH2:19][CH3:18])[C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[C:5]1=[O:17])(=[O:3])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 74268Benzene, (triethoxymethyl)-HCID 226685441-Acetyl-5,6-dimethoxy-2-indolinone

生成物 1

HCID 695643221-Acetyl-3-(1-ethoxy-1-phenylmethylidene)-5,6-dimethoxy-2-indolinone

試薬・触媒・溶媒 1

HCID 7918Acetic Anhydride溶媒

実験手順

10.0 g of 1-acetyl-5,6-dimethoxy-2-indolinone, 29.2 ml of triethyl orthobenzoate and 100 ml of acetic anhydride are stirred for 48 hours at 120° C. The solvent is eliminated and the residue evaporated with toluene, combined with ether and the precipitate formed (starting compounds is suction filtered. The filtrate is concentrated by evaporation and separated through a silica gel column with toluene, then with toluene/ethyl acetate (10:1). The product is triturated with ether, suction filtered and dried in vacuo at 100° C.

後処理

  1. customthe residue evaporated with toluene
  2. customthe precipitate formed (
  3. filtrationfiltered
  4. concentrationThe filtrate is concentrated by evaporation
  5. customseparated through a silica gel column with toluene
  6. customThe product is triturated with ether, suction
  7. filtrationfiltered
  8. customdried in vacuo at 100° C.

出典と根拠

ORDレコード
ord-a702140750b24dcc85f451cc428b390a
出典データセット
uspto-grants-2004_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06794395B1

反応ノート

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