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Isopropanol → [7-(benzyloxy)-5-isopropoxy-4-oxoquinazolin-3(4H)-yl]methyl pivalate

HRID 639979
ノート
印刷プレビュー

反応式

HRID 639979 の反応式
[CH:1](O)([CH3:3])[CH3:2].[C:5]([O:11][CH2:12][N:13]1[C:22](=[O:23])[C:21]2[C:16](=[CH:17][C:18]([O:25][CH2:26][C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=3)=[CH:19][C:20]=2[OH:24])[N:15]=[CH:14]1)(=[O:10])[C:6]([CH3:9])([CH3:8])[CH3:7].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.CC(OC(/N=N/C(OC(C)(C)C)=O)=O)(C)C>ClCCl>[C:5]([O:11][CH2:12][N:13]1[C:22](=[O:23])[C:21]2[C:16](=[CH:17][C:18]([O:25][CH2:26][C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=3)=[CH:19][C:20]=2[O:24][CH:1]([CH3:3])[CH3:2])[N:15]=[CH:14]1)(=[O:10])[C:6]([CH3:9])([CH3:8])[CH3:7]
参加物反応条件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 3776IsopropanolHCID 11776TriphenylphosphineHCID 6034084Di-tert-butyl diazene-1,2-dicarboxylateHCID 119746277-Benzyloxy-5-hydroxy-3-pivaloyloxymethyl-3,4-dihydroquinazolin-4-one

生成物 1

HCID 68639837[7-(benzyloxy)-5-isopropoxy-4-oxoquinazolin-3(4H)-yl]methyl pivalate

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒
2 回

反応条件

温度
0 °C

実験手順

Isopropanol (1.5 ml, 18.7 mmol) was added to a solution of [7-(benzyloxy)-5-hydroxy-4-oxoquinazolin-3(4H)-yl]methyl pivalate (see WO01/094341, 6.5 g, 17.0 mmol) and triphenylphosphine (6.2 g, 23.8 mmol) in dichloromethane (300 ml). The reaction mixture was cooled to 0° C. and then a solution of di-tert-butylazodicarboxylate (4.7 g, 20.4 mmol) in dichloromethane (25 ml) was added dropwise over 30 minutes. The mixture was allowed to warm to room temperature and then stirred for 2 hours. The mixture was evaporated under reduced pressure to afford crude [7-(benzyloxy)-5-isopropoxy-4-oxoquinazolin-3(4H)-yl]methyl pivalate which was used in the next stage without further purification.

後処理

  1. temperatureto warm to room temperature
  2. customThe mixture was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-a4c7d538fe784cdab6ba7041f3d71357
出典データセット
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07691867B2

反応ノート

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