Triethylamine → HCID 20306069, 화합물

HRID 1732400

반응식

HRID 1732400 반응식
[C:1]1([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH:6]=[CH:5][C:4]([O:7][CH:8]([N:15]2[CH:19]=[N:18][CH:17]=[N:16]2)[CH:9]([OH:14])[C:10]([CH3:13])([CH3:12])[CH3:11])=[CH:3][CH:2]=1.[CH3:26][O:27][CH2:28][N:29]=[C:30]=[O:31].C(N(CC)CC)C.C([O-])(=O)CCCCCCCCCCC.C([O-])(=O)CCCCCCCCCCC.C([Sn+2]CCCC)CCC>O1CCCC1>[C:1]1([C:20]2[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=2)[CH:6]=[CH:5][C:4]([O:7][CH:8]([N:15]2[CH:19]=[N:18][CH:17]=[N:16]2)[CH:9]([O:14][C:30](=[O:31])[NH:29][CH2:28][O:27][CH3:26])[C:10]([CH3:13])([CH3:12])[CH3:11])=[CH:3][CH:2]=1

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 62609Methoxymethyl isocyanateHCID 91656BitertanolHCID 9809426Di-n-butyldilauryltin

생성물 1

HCID 20306069HCID 20306069, 화합물수율 82.9%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

505 g (1.5 moles) of 1-(4-biphenylyloxy)-3,3-dimethyl-1-(1,2,4-triazol-1-yl)-butan-2-ol (A form) and 140 g (1.6 moles) of methoxymethyl isocyanate were heated under reflux in 2.5 liters of tetrahydrofuran in the presence of 40 ml of triethylamine and 1 ml of dibutyl-tin dilaurate for 48 hours. Thereafter, the solvent was stripped off in vacuo and 3 liters of petroleum ether were added to the residue. The crystalline precipitate formed was extracted by stirring with 1.5 liters of diisopropyl ether. 528 g (82.5% of theory) of 1-(4-biphenylyloxy)-3,3-dimethyl-2-methoxymethylcarbamoyloxy-1-(1,2,4-triazol-1-yl)-butane (A form) of melting point 95°-98° C. were obtained.

후처리

  1. additionwere added to the residue
  2. customThe crystalline precipitate formed
  3. extractionwas extracted

출처 및 근거

ORD 기록
ord-241dca38976241c782d44dc4f4610135
출처 데이터셋
uspto-grants-1980_12
특허 번호
US04237142

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