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Dichloromethane → 4-(4-Bromo-2-fluoroanilino)-7-(3-(1,1-dioxothiomorpholino)propoxy)-6-methoxyquinazoline hydrochloride

HRID 547232
ノート
印刷プレビュー

反応式

HRID 547232 の反応式
N(C(OCC)=O)=NC(OCC)=O.[Br:13][C:14]1[CH:33]=[CH:32][C:17]([NH:18][C:19]2[C:28]3[C:23](=[CH:24][C:25]([OH:31])=[C:26]([O:29][CH3:30])[CH:27]=3)[N:22]=[CH:21][N:20]=2)=[C:16]([F:34])[CH:15]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[O:54]=[S:55]1(=[O:65])[CH2:60][CH2:59][N:58]([CH2:61][CH2:62][CH2:63]O)[CH2:57][CH2:56]1.C(Cl)[Cl:67]>>[ClH:67].[Br:13][C:14]1[CH:33]=[CH:32][C:17]([NH:18][C:19]2[C:28]3[C:23](=[CH:24][C:25]([O:31][CH2:63][CH2:62][CH2:61][N:58]4[CH2:57][CH2:56][S:55](=[O:65])(=[O:54])[CH2:60][CH2:59]4)=[C:26]([O:29][CH3:30])[CH:27]=3)[N:22]=[CH:21][N:20]=2)=[C:16]([F:34])[CH:15]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 5

HCID 6344DichloromethaneHCID 11776Triphenylphosphine2 回HCID 220568ethyl N-ethoxycarbonyliminocarbamate2 回HCID 114354734-(3-Hydroxypropyl)thiomorpholine 1,1-Dioxide2 回HCID 1355038524-[(4-Bromo-2-fluorophenyl)amino]-6-methoxy-7-quinazolinol

生成物 1

HCID 67045152
4-(4-Bromo-2-fluoroanilino)-7-(3-(1,1-dioxothiomorpholino)propoxy)-6-methoxyquinazoline hydrochloride
収率 47%

実験手順

Diethyl azodicarboxylate (220 μl, 1.4 mmol) was added dropwise to a mixture of 4-(4-bromo-2-fluoroanilino)-7-hydroxy-6-methoxyquinazoline (170 mg, 0.46 mmol), (prepared as described for the starting material in Example 48), triphenylphosphine (367 mg, 1.4 mmol) and 3-(1,1-dioxothiomorpholino)-1-propanol (135 mg, 0.7 mmol) in methylene chloride (4 ml) under nitrogen. The mixture was stirred for 1 hour at ambient temperature and further triphenylphosphine (61 mg, 0.23 mmol), 3-(1,1-dioxothiomorpholino)-1-propanol (30 mg, 0.23 mmol) and diethyl azodicarboxylate (37 μl, 0.23 mmol) were added. The mixture was stirred for 1 hour at ambient temperature and the mixture was purified by pouring it on to a column of silica and eluting with methylene chloride/methanol (95/5). The purified product was dissolved in methylene chloride/methanol, 2.2M ethereal hydrogen chloride (1 ml) was added and the volatiles were removed by evaporation. The residue was triturated with ether, collected by filtration, washed with ether and dried under vacuum to give 4-(4-bromo-2-fluoroanilino)-7-(3-(1,1-dioxothiomorpholino)propoxy)-6-methoxyquinazoline hydrochloride (138 mg, 47%).

後処理

  1. custom(prepared
  2. stirringThe mixture was stirred for 1 hour at ambient temperature
  3. customthe mixture was purified
  4. additionby pouring it on to a column of silica
  5. washeluting with methylene chloride/methanol (95/5)
  6. dissolutionThe purified product was dissolved in methylene chloride/methanol
  7. addition2.2M ethereal hydrogen chloride (1 ml) was added
  8. customthe volatiles were removed by evaporation
  9. customThe residue was triturated with ether
  10. filtrationcollected by filtration
  11. washwashed with ether
  12. customdried under vacuum

出典と根拠

ORDレコード
ord-1911cdf7bac34bf0b8103c5d8e2c3d1e
出典データセット
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
USRE042353E1

反応ノート

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