Diisopropyl Ether → 5-Nitro-2-pyrrolidin-1-ylmethylbenzoxazole

HRID 735100

反応式

HRID 735100 の反応式
Cl[CH2:2][C:3]1[O:4][C:5]2[CH:11]=[CH:10][C:9]([N+:12]([O-:14])=[O:13])=[CH:8][C:6]=2[N:7]=1.[NH:15]1[CH2:19][CH2:18][CH2:17][CH2:16]1.C(=O)([O-])[O-].[K+].[K+].C(OC(C)C)(C)C>CN(C=O)C.O>[N+:12]([C:9]1[CH:10]=[CH:11][C:5]2[O:4][C:3]([CH2:2][N:15]3[CH2:19][CH2:18][CH2:17][CH2:16]3)=[N:7][C:6]=2[CH:8]=1)([O-:14])=[O:13]

参加物

7

反応物 4

HCID 7914Diisopropyl EtherHCID 11430Potassium CarbonateHCID 31268PyrrolidineHCID 27641892-(Chloromethyl)-5-nitro-1,3-benzoxazole

生成物 1

HCID 597669925-Nitro-2-pyrrolidin-1-ylmethylbenzoxazole

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
50 °C

実験手順

A reaction mixture of 3 g (14.11 mmol) of 2-chloromethyl-5-nitrobenzoxazole, 1.5 mL (17.97 mmol) of pyrrolidine, and 3.9 g (28.22 mmol) of potassium carbonate in 30 mL of DMF is stirred for 4 hours at 50° C. Then the reaction mixture is diluted with water and covered with diisopropyl ether, The precipitated yellow solid is suction filtered, washed again, and dried in the circulating air dryer at 60° C. Yield: 1.8 g (52% of theory); C12H13N3O3 (M=247.25); calc.: molecular ion peak (M+H)+: 248; found: molecular ion peak (M+H)+: 248; Rf value: 0.4 (silica gel, dichloromethane/ethanol (20:1)).

後処理

  1. filtrationfiltered
  2. washwashed again
  3. customdried in the circulating air dryer at 60° C

出典と根拠

ORDレコード
ord-652e8ce8327f40859f9e5f8de2b56507
出典データセット
uspto-grants-2009_09
特許番号
US07592373B2

関連ノート

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