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Methyl10-methoxymethyl-10H-pyrazino[2,3-b][1,4]benzothiazine-8-carboxylate → 10-Methoxymethyl-10H-pyrazino[2,3-b][1,4]benzothiazine-8-methanol

HRID 1059275
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HRID 1059275 반응식
[CH3:1][O:2][CH2:3][N:4]1[C:9]2[CH:10]=[C:11]([C:14](OC)=[O:15])[CH:12]=[CH:13][C:8]=2[S:7][C:6]2[N:18]=[CH:19][CH:20]=[N:21][C:5]1=2.[H-].C([Al+]CC(C)C)C(C)C>C(Cl)Cl.C1(C)C=CC=CC=1>[CH3:1][O:2][CH2:3][N:4]1[C:9]2[CH:10]=[C:11]([CH2:14][OH:15])[CH:12]=[CH:13][C:8]=2[S:7][C:6]2[N:18]=[CH:19][CH:20]=[N:21][C:5]1=2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 11472176Methyl10-methoxymethyl-10H-pyrazino[2,3-b][1,4]benzothiazine-8-carboxylateHCID 21225700Diisobutylaluminumhydride

생성물 1

HCID 1126581710-Methoxymethyl-10H-pyrazino[2,3-b][1,4]benzothiazine-8-methanol수율 78.7%

시약·촉매·용매 2

HCID 1140Toluene용매HCID 6344Dichloromethane용매

실험 절차

Into a solution of 350 g of methyl 10-methoxymethyl-10H-pyrazino[2,3-b][1,4]benzothiazine-8-carboxylate in methylene chloride (2.5 l) was added dropwise under a nitrogen atmosphere 3.2 l of a 1.01 M solution of diisobutylaluminum hydride in toluene while maintaining the system at a temperature not exceeding 15° C. Then the reaction mixture was poured into ice and stirred for 1 hour. After filtering off the insoluble matter, the filtrate was washed with water. After distilling off the solvent under reduced pressure, the crude crystals thus obtained were washed with diisopropyl ether to thereby give 250 g of the title compound as pale yellow crystals.

후처리

  1. temperaturewhile maintaining the system at a temperature not
  2. customexceeding 15° C
  3. additionThen the reaction mixture was poured into ice
  4. filtrationAfter filtering off the insoluble matter
  5. washthe filtrate was washed with water
  6. distillationAfter distilling off the solvent under reduced pressure
  7. customthe crude crystals thus obtained
  8. washwere washed with diisopropyl ether

출처 및 근거

ORD 기록
ord-87a29f1adeb04f6f9b3bd44ca5e953f6
출처 데이터셋
uspto-grants-2003_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06518423B1

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