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Phthalimide → N-(10-Methoxymethyl-10H-pyrazino[2,3-b][1,4]benzothiazin-8-ylmethyl)phthalimide

HRID 1059423
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인쇄 미리보기

반응식

HRID 1059423 반응식
[CH3:1][O:2][CH2:3][N:4]1[C:9]2[CH:10]=[C:11]([CH2:14]O)[CH:12]=[CH:13][C:8]=2[S:7][C:6]2[N:16]=[CH:17][CH:18]=[N:19][C:5]1=2.[C:20]1(=[O:30])[NH:24][C:23](=[O:25])[C:22]2=[CH:26][CH:27]=[CH:28][CH:29]=[C:21]12.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.N(C(OCC)=O)=NC(OCC)=O>O1CCCC1>[CH3:1][O:2][CH2:3][N:4]1[C:9]2[CH:10]=[C:11]([CH2:14][N:24]3[C:23](=[O:25])[C:22]4=[CH:26][CH:27]=[CH:28][CH:29]=[C:21]4[C:20]3=[O:30])[CH:12]=[CH:13][C:8]=2[S:7][C:6]2[N:16]=[CH:17][CH:18]=[N:19][C:5]1=2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 6809PhthalimideHCID 11776TriphenylphosphineHCID 220568ethyl N-ethoxycarbonyliminocarbamateHCID 1126581710-Methoxymethyl-10H-pyrazino[2,3-b][1,4]benzothiazine-8-methanol

생성물 1

HCID 18670612N-(10-Methoxymethyl-10H-pyrazino[2,3-b][1,4]benzothiazin-8-ylmethyl)phthalimide수율 53.3%

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매

실험 절차

A solution of 3.32 g of (10-methoxymethyl-10H-pyrazino[2,3-b][1,4]benzothiazin-8-yl)methanol, 2.12 g of phthalimide and 3.77 g of triphenylphosphine in tetrahydrofuran (50 ml) was ice-cooled and 2.24 ml of diethyl azodicarboxylate was dropped thereinto. After stirring at room temperature for 1 hour, the solvent was distilled off under reduced pressure and diethyl ether was added to the residue. Then it was subjected to ultrasonication and the crystals thus precipitated were taken up by filtration to thereby give 2.6 g of the title compound as pale yellow crystals.

후처리

  1. temperaturecooled
  2. distillationthe solvent was distilled off under reduced pressure and diethyl ether
  3. additionwas added to the residue
  4. customThen it was subjected to ultrasonication
  5. customthe crystals thus precipitated
  6. filtrationwere taken up by filtration

출처 및 근거

ORD 기록
ord-9bb989bb16214cebb991b4fffb7dc45c
출처 데이터셋
uspto-grants-2003_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06518423B1

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