Sodium hydride → HCID 14402884, 화합물

HRID 1381819노트

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HRID 1381819 반응식
[H-].[Na+].[F:3][C:4]1[C:14]([N:15]2[C:23](=[O:24])[C:22]3[CH2:21][CH2:20][CH2:19][CH2:18][C:17]=3[C:16]2=[O:25])=[CH:13][C:7]2[NH:8][C:9](=[O:12])[CH2:10][O:11][C:6]=2[CH:5]=1.Cl[CH2:27][Si:28]([CH3:31])([CH3:30])[CH3:29]>CN(C)C=O.[I-].[Na+].C1OCCOCCOCCOCCOCCOC1>[F:3][C:4]1[C:14]([N:15]2[C:23](=[O:24])[C:22]3[CH2:21][CH2:20][CH2:19][CH2:18][C:17]=3[C:16]2=[O:25])=[CH:13][C:7]2[N:8]([CH2:27][Si:28]([CH3:31])([CH3:30])[CH3:29])[C:9](=[O:12])[CH2:10][O:11][C:6]=2[CH:5]=1

참가 물질

7

반응물 3

HCID 24758Sodium hydrideHCID 75361Silane, (chloromethyl)trimethyl-HCID 137721852-(7-Fluoro-3-oxo-4H-1,4-benzoxazin-6-yl)-4,5,6,7-tetrahydroisoindole-1,3-dione

생성물 1

HCID 14402884HCID 14402884, 화합물수율 87.3%

시약·촉매·용매 3

HCID 5238Sodium Iodide촉매HCID 2855718-Crown-6촉매HCID 6228Dimethylformamide용매2회

실험 절차

To N,N-dimethylformamide (10 ml) is added at an ambient temperature sodium hydride (0.1 g), sodium iodide (5 mg), 18-crown-6 (5 mg) and 2-[7-fluoro-2H-1,4-benzoxazin-3(4H)-on-6-yl]-4,5,6,7-tetrahydro-2H-isoindole-1,3-dione (0.63 g). Thereafter the whole is stirred for 15 minutes, treated with a solution of chloromethyltrimethylsilane (0.61 g) in N,N-dimethylformamide (5 ml), and stirred at 100°-110° C. for an hour. The reaction mixture is evaporated to dryness in vacuo, admixed with water (30 ml), and extracted twice with dichloromethane (30 ml). The combined extract is dried over sodium sulfate and evaporated in vacuo to obtain an oily end product 2-[7-fluoro-4-trimethylsilylmethyl-2H-1,4-benzoxazin-3(4H)-on-6-yl]-4,5,6,7-tetrahydro-2H-isoindole-1,3-dione (0.7 g). nD20 1.5596.

후처리

  1. stirringstirred at 100°-110° C. for an hour
  2. customThe reaction mixture is evaporated to dryness in vacuo
  3. extractionextracted twice with dichloromethane (30 ml)
  4. extractionThe combined extract
  5. dry with materialis dried over sodium sulfate
  6. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-8bbc8ba8f2d648ea87511a5ef7a4723a
출처 데이터셋
uspto-grants-1989_02
특허 번호
US04804394

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