Sodium hydride → HCID 14402884、化合物

HRID 1381819ノート

反応式

HRID 1381819 の反応式
[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

参加物

7

反応物 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

生成物 1

HCID 14402884HCID 14402884、化合物収率 87.3%

試薬・触媒・溶媒 3

HCID 5238Sodium Iodide触媒HCID 2855718-Crown-6触媒HCID 6228Dimethylformamide溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8bbc8ba8f2d648ea87511a5ef7a4723a
出典データセット
uspto-grants-1989_02
特許番号
US04804394

反応ノート

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