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Triphenylphosphine → HCID 70099554、化合物

HRID 1737622
ノート
印刷プレビュー

反応式

HRID 1737622 の反応式
N(C(OCC)=O)=NC(OCC)=O.[Cl: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.[CH3:35][C:36]1[N:40]([CH2:41][CH2:42]O)[C:39]([CH3:44])=[N:38][N:37]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>C(Cl)Cl>[ClH:13].[Cl: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][CH2:42][CH2:41][N:40]4[C:39]([CH3:44])=[N:38][N:37]=[C:36]4[CH3:35])=[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 4

HCID 11776TriphenylphosphineHCID 220568ethyl N-ethoxycarbonyliminocarbamateHCID 20026677HCID 20026677、化合物HCID 1355137204-(4-Chloro-2-fluorophenylamino)-7-hydroxy-6-methoxyquinazoline

生成物 1

HCID 70099554HCID 70099554、化合物収率 123.8%

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒

実験手順

Diethyl azodicarboxylate (295 μl, 1. 8 mmol) was added dropwise to a suspension of 4-(4-chloro-2-fluoroanilino)-7-hydroxy-6-methoxyquinazoline (200 mg, 0.62 mmol), (prepared as described for the starting material in Example 24), 2-(3,5-dimethyl-[1,2,4]-triazol-4-yl)ethanol (114 mg, 0.81mmol), (EP 0329357 A1), and triphenylphosphine (492 mg, 1.8 mmol) in methylene chloride (4 ml) and the mixture stirred for 1 hour at ambient temperature. The precipitated solid was collected by filtration, washed with ether and dried under vacuum. The solid was dissolved in methylene chloride/methanol and ethereal hydrogen chloride (2 ml of 4.5M solution) was added. The volatiles were removed by evaporation, the residue was suspended in ether, collected by filtration, washed with ether and dried under vacuum to give 4-(4-chloro-2-fluoroanilino)-7-(2-(3,5-dimethyl-[1,2,4]-triazol-4-yl)ethoxy)-6-methoxyquinazoline hydrochloride (184 mg, 54%).

後処理

  1. custom(prepared
  2. filtrationThe precipitated solid was collected by filtration
  3. washwashed with ether
  4. customdried under vacuum
  5. dissolutionThe solid was dissolved in methylene chloride/methanol
  6. additionethereal hydrogen chloride (2 ml of 4.5M solution) was added
  7. customThe volatiles were removed by evaporation
  8. filtrationcollected by filtration
  9. washwashed with ether
  10. customdried under vacuum

出典と根拠

ORDレコード
ord-12964da941114e2abdc4461878a4ba7f
出典データセット
uspto-grants-1999_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05962458

反応ノート

読み込み中…

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