Phosphoric Acid → HCID 86722238、化合物

HRID 869389ノート

反応式

HRID 869389 の反応式
[NH2:1][C:2]1[C:6]2[C:7]([Cl:13])=[C:8]([O:11][CH3:12])[CH:9]=[CH:10][C:5]=2[O:4][C:3]=1[C:14](=[O:25])/[CH:15]=[CH:16]/[C:17]1[S:21][C:20]([CH:22]([CH3:24])[CH3:23])=[N:19][CH:18]=1.CC#N.OP(O)(O)=O>[Cl-].[Cl-].[Zn+2].CC(O)=O>[Cl:13][C:7]1[C:6]2[C:2]3[NH:1][CH:16]([C:17]4[S:21][C:20]([CH:22]([CH3:23])[CH3:24])=[N:19][CH:18]=4)[CH2:15][C:14](=[O:25])[C:3]=3[O:4][C:5]=2[CH:10]=[CH:9][C:8]=1[O:11][CH3:12]

参加物

6

反応物 3

HCID 1004Phosphoric AcidHCID 6342AcetonitrileHCID 86722237HCID 86722237、化合物

生成物 1

HCID 86722238HCID 86722238、化合物収率 68.6%

試薬・触媒・溶媒 2

HCID 3007855Zincchloride触媒HCID 176Acetic Acid溶媒

実験手順

9A (3.5 g, 9.28 mmol) was added to MeCN (50 mL) and stirred at room temperature. To the mixture was added ZnCl2 (1.91 g, 13.93 mmol, 1.5 eq), followed by AcOH (50 mL) and H3PO4 (50 mL) The reaction mixture was heated to 80° C. and stirred overnight. After reaction completed, the mixture was cooled and poured into crushed ice under stirring, neutralized to pH=7˜8, extracted with ethyl acetate, dried and concentrated to give 2.4 g of product (9B).

後処理

  1. temperaturewas heated to 80° C.
  2. stirringstirred overnight
  3. customAfter reaction
  4. temperaturethe mixture was cooled
  5. additionpoured
  6. custominto crushed ice
  7. stirringunder stirring
  8. extractionextracted with ethyl acetate
  9. customdried
  10. concentrationconcentrated

出典と根拠

ORDレコード
ord-cb3a3555d48746bb9b7a6c3cb05bee96
出典データセット
uspto-grants-2015_03
特許番号
US08969373B2

反応ノート

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