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Acetic Anhydride → 4-(4-Chloro-3-formamidobenzyl)amino-6-chloroquinazoline

HRID 1003525
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인쇄 미리보기

반응식

HRID 1003525 반응식
[NH2:1][C:2]1[CH:3]=[C:4]([CH:18]=[CH:19][C:20]=1[Cl:21])[CH2:5][NH:6][C:7]1[C:16]2[C:11](=[CH:12][CH:13]=[C:14]([Cl:17])[CH:15]=2)[N:10]=[CH:9][N:8]=1.[C:22](OC(=O)C)(=[O:24])C>C(O)=O>[Cl:21][C:20]1[CH:19]=[CH:18][C:4]([CH2:5][NH:6][C:7]2[C:16]3[C:11](=[CH:12][CH:13]=[C:14]([Cl:17])[CH:15]=3)[N:10]=[CH:9][N:8]=2)=[CH:3][C:2]=1[NH:1][CH:22]=[O:24]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 7918Acetic AnhydrideHCID 187967134-(3-Amino-4-chlorobenzyl)amino-6-chloroquinazoline

생성물 1

HCID 187966694-(4-Chloro-3-formamidobenzyl)amino-6-chloroquinazoline수율 65%

시약·촉매·용매 1

HCID 284Formic Acid용매

실험 절차

0.90 g (2.82 mmol) of the 4-(3-amino-4-chlorobenzyl)amino-6-chloroquinazoline prepared in Example 147 was dissolved in 15 ml of formic acid, followed by the addition of 1 ml of acetic anhydride. The obtained mixture was stirred at room temperature for several hours and distilled under a reduced pressure to remove the solvent. The residue was purified by silica gel column chromatography (ethyl acetate) and recrystallized from ethyl acetate to give 0.64 g of the title compound as a pale yellow crystal.

후처리

  1. distillationdistilled under a reduced pressure
  2. customto remove the solvent
  3. customThe residue was purified by silica gel column chromatography (ethyl acetate)
  4. customrecrystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-773caab339234b1d9fde1ccb798956fb
출처 데이터셋
uspto-grants-2000_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06046206

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