Hexamethyldisilazane → HCID 178451017, 화합물

HRID 842590

반응식

HRID 842590 반응식
[PH2:1](=[O:3])[O-:2].[NH4+].C[Si](C)(C)N[Si](C)(C)C.[CH2:14]=[C:15]([CH2:23][CH2:24][C:25]([O:27][C:28]([CH3:31])([CH3:30])[CH3:29])=[O:26])[C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17]>ClCCl>[OH:3][PH:1]([CH2:14][CH:15]([CH2:23][CH2:24][C:25]([O:27][C:28]([CH3:29])([CH3:31])[CH3:30])=[O:26])[C:16]([O:18][C:19]([CH3:20])([CH3:21])[CH3:22])=[O:17])=[O:2]

참가 물질

5

반응물 3

HCID 13838HexamethyldisilazaneHCID 11054274Di-tert-butyl 2-methylenepentanedioateHCID 178418291HCID 178418291, 화합물

생성물 1

HCID 178451017HCID 178451017, 화합물수율 100%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
105 °C

실험 절차

A mixture of ammonium phosphinate (162.6 g, 1.96 mol) and 1,1,1,3,3,3-hexamethyldisilazane (316 g, 1.96 mol) was heated to 105° C. for 2 hours. The reaction mixture was cooled in an ice bath and di-tert-butyl 2-methylenepentane-1,5-dioate (251 g, 0.979 mol) dissolved in dichloromethane (1000 ml) was added dropwise. The reaction mixture was allowed to warm to room temperature overnight. The reaction mixture was then quenched with distilled water (500 ml) and the organic layer was retained. The aqueous layer was washed a second time with dichloromethane and the combined organic layers were dried over magnesium sulfate. Then the solvent was removed under reduced pressure leaving a slightly yellow oil (315 g, 100%) This product was found to be of sufficient purity for use in the next reaction. 1H NMR (CDCl3): δ1.4 (m, 18H), 1.9 (m, 3H), 2.1 (m, 1H), 2.3 (m, 2H), 2.7 (m, 1H), 6.5 & 7.9 (d, 1H, the P—H), 11.0 (s, 1H).

후처리

  1. temperatureThe reaction mixture was cooled in an ice bath
  2. additionwas added dropwise
  3. temperatureto warm to room temperature overnight
  4. customThe reaction mixture was then quenched with distilled water (500 ml)
  5. washThe aqueous layer was washed a second time with dichloromethane
  6. dry with materialthe combined organic layers were dried over magnesium sulfate
  7. customThen the solvent was removed under reduced pressure

출처 및 근거

ORD 기록
ord-a707836626d44edfbe16c216d186f056
출처 데이터셋
uspto-grants-2002_04
특허 번호
US06376478B1

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