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Ethyl Acetoacetate → HCID 19967112、化合物

HRID 2081613
ノート
印刷プレビュー

反応式

HRID 2081613 の反応式
[N:1]1([CH2:6][C:7]2[CH:12]=[CH:11][C:10]([NH2:13])=[CH:9][CH:8]=2)[CH:5]=[CH:4][N:3]=[CH:2]1.O=[C:15]([CH3:22])[CH2:16][C:17](OCC)=[O:18].C(=O)([O-])[O-].[K+].[K+]>O>[N:1]1([CH2:6][C:7]2[CH:12]=[C:11]3[C:10](=[CH:9][CH:8]=2)[NH:13][C:15]([CH3:22])=[CH:16][C:17]3=[O:18])[CH:5]=[CH:4][N:3]=[CH:2]1
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 8868Ethyl AcetoacetateHCID 11430Potassium CarbonateHCID 12653191-(4-Aminobenzyl)-1H-imidazole

生成物 1

HCID 19967112HCID 19967112、化合物収率 14.4%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a stirred and heated (100° C.) solution of 10 parts of 4-(1H-imidazol-1-ylmethyl)benzenamine in 50 parts of poly phosphoric acid were added 15 parts of ethyl 3-oxobutanoate. The whole was stirred for 4 hours at 140° C. 100 Parts of water were added to the mixture and the whole was neutralized with potassium carbonate. The product was extracted with a mixture of ethyl acetate and methanol. The extract was dried, filtered and concentrated. The concentrate was crystallized from a mixture of 2-propanone and methanol. The product was filtered off and dried, yielding 2 parts (14.4%) of 6-(1H-imidazol-1-ylmethyl)-2-methyl-4(1H)quinolinone; mp. 245.5° C. (decomp.) (compound 51).

後処理

  1. stirringThe whole was stirred for 4 hours at 140° C
  2. extractionThe product was extracted with a mixture of ethyl acetate and methanol
  3. customThe extract was dried
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customThe concentrate was crystallized from a mixture of 2-propanone and methanol
  7. filtrationThe product was filtered off
  8. customdried

出典と根拠

ORDレコード
ord-e040385ec0cc4ae1aa919561251e0321
出典データセット
uspto-grants-1993_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05185346

反応ノート

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