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

HRID 735100

반응식

HRID 735100 반응식
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]

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

반응 조건

온도
50 °C

실험 절차

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)).

후처리

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

출처 및 근거

ORD 기록
ord-652e8ce8327f40859f9e5f8de2b56507
출처 데이터셋
uspto-grants-2009_09
특허 번호
US07592373B2

연결된 노트

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