Phosphoric Acid → HCID 86722238, 화합물

HRID 869389노트

반응식

HRID 869389 반응식
[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]

참가 물질

6

반응물 3

HCID 1004Phosphoric AcidHCID 6342AcetonitrileHCID 86722237HCID 86722237, 화합물

생성물 1

HCID 86722238HCID 86722238, 화합물수율 68.6%

시약·촉매·용매 2

HCID 3007855Zincchloride촉매HCID 176Acetic Acid용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-cb3a3555d48746bb9b7a6c3cb05bee96
출처 데이터셋
uspto-grants-2015_03
특허 번호
US08969373B2

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