tert-Butyl methyl ether → Didodecyl 2-(t-butylthio)-1-hydroxy-1-methylethanephosphonate

HRID 1079098노트

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HRID 1079098 반응식
[P:1]([O-:28])([O:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH3:27])[O:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH3:14].COC(C)(C)C.N12CCCNC1C=CCCC2.[C:46]([S:50][CH2:51][C:52](=[O:54])[CH3:53])([CH3:49])([CH3:48])[CH3:47]>C1(C)C=CC=CC=1.CS(C)=O>[C:46]([S:50][CH2:51][C:52]([OH:54])([CH3:53])[P:1]([O:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH3:27])(=[O:28])[O:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH3:14])([CH3:49])([CH3:48])[CH3:47]

참가 물질

7

반응물 4

HCID 15413tert-Butyl methyl etherHCID 114236691-(Tert-butylsulfanyl)propan-2-oneHCID 150726561,2,3,4,6,7,8,10A-octahydropyrimido[1,2-a]azepineHCID 21884946CID 21884946

생성물 1

HCID 19428699Didodecyl 2-(t-butylthio)-1-hydroxy-1-methylethanephosphonate

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 1140Toluene용매

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온도
60 °C

실험 절차

23.0 g (55 mmol) of didodecyl phosphite are initially introduced into a mixture of 20 ml of tert-butyl methyl ether and 5 ml of dimethyl sulfoxide. 1.0 g of 1,8-diazabicyclo[5.4.0]undec-5-ene (DBU) are added, and 8.04 g (55 mmol) of (t-butylthio)acetone are then added dropwise at 30° C. The reaction mixture is heated for 5 hours at 60° C., cooled, diluted with 150 ml of toluene and washed with 100 ml of water. The organic phase is dried over sodium sulfate, and the solvent and remainders of the educts are distilled off in vacuo (finally at 0.5 mbar and 55° C. bath temperature).

후처리

  1. temperaturecooled
  2. washwashed with 100 ml of water
  3. dry with materialThe organic phase is dried over sodium sulfate
  4. distillationthe solvent and remainders of the educts are distilled off in vacuo (finally at 0.5 mbar and 55° C. bath temperature)

출처 및 근거

ORD 기록
ord-b5843fedb2dc44da9fcd9d43da58a25d
출처 데이터셋
uspto-grants-1996_08
특허 번호
US05550276

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