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

HRID 1079098ノート

反応式

HRID 1079098 の反応式
[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]

参加物

7

反応物 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

生成物 1

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

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒HCID 1140Toluene溶媒

反応条件

温度
60 °C

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-b5843fedb2dc44da9fcd9d43da58a25d
出典データセット
uspto-grants-1996_08
特許番号
US05550276

反応ノート

読み込み中…