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Hydrochloric Acid → HCID 13557219, 화합물

HRID 1583477
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HRID 1583477 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([NH:8]C(OCC)=O)[CH:5]=[CH:4][C:3]=1[CH2:14][N:15]1[C:19](=[O:20])[C:18]([CH3:22])([CH3:21])[CH2:17][O:16]1.I[Si](C)(C)C.Cl>C(Cl)(Cl)Cl>[NH2:8][C:6]1[CH:5]=[CH:4][C:3]([CH2:14][N:15]2[C:19](=[O:20])[C:18]([CH3:21])([CH3:22])[CH2:17][O:16]2)=[C:2]([Cl:1])[CH:7]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 85247Trimethylsilyl iodideHCID 13557218HCID 13557218, 화합물

생성물 1

HCID 13557219HCID 13557219, 화합물

시약·촉매·용매 1

HCID 6212Chloroform용매

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온도
60 °C

실험 절차

To a stirred suspension of 8.4 grams (0.026 mole) of 2-[2-chloro-4-(ethoxycarbonylamino)phenyl]methyl-4,4-dimethyl-3-isoxazolidinone in 100 ml of chloroform, under an argon atmosphere and at ambient temperature, was carefully added dropwise 6.0 grams (0.03 mole) of iodotrimethylsilane. Upon completion of addition the reaction mixture was warmed to 60° C. where it stirred for 16 hours. Five ml of methanolic 2N hydrochloric acid was added to the reaction mixture. The solution was stirred for 10 minutes, then concentrated under reduced pressure to a residual solid. The solid was triturated in 25 ml of water. The water/solid mixture was neutralized with aqueous saturated sodium bicarbonate solution. The solid was collected by filtration to give 2-(4-amino-2-chlorophenyl)methyl-4,4-dimethyl-3-isoxazolidinone; m.p. 106°-108° C.

후처리

  1. additionUpon completion of addition the reaction mixture
  2. stirringThe solution was stirred for 10 minutes
  3. concentrationconcentrated under reduced pressure to a residual solid
  4. customThe solid was triturated in 25 ml of water
  5. filtrationThe solid was collected by filtration

출처 및 근거

ORD 기록
ord-3ce45752126b4e3d81325025a5985e72
출처 데이터셋
uspto-grants-1985_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04552585

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