Triethylamine → N-carbomethoxy-N'-benzylsulfamoyl-O-methylisourea

HRID 1982166노트

반응식

HRID 1982166 반응식
[CH2:1]([NH:8][S:9](Cl)(=[O:11])=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:13]([NH:17][C:18](=[NH:21])[O:19][CH3:20])([O:15][CH3:16])=[O:14].C(N(CC)CC)C>C1COCC1>[C:13]([NH:17][C:18](=[N:21][S:9](=[O:11])(=[O:10])[NH:8][CH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)[O:19][CH3:20])([O:15][CH3:16])=[O:14]

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 13529095Benzylsulfamyl chlorideHCID 137319931Methyl N-(iminomethoxymethyl)carbamate

생성물 1

HCID 70392213N-carbomethoxy-N'-benzylsulfamoyl-O-methylisourea

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of benzylsulfamoyl chloride (168 g) in anhydrous THF (300 ml) is added dropwise to a stirred solution of N-carbomethoxy-O-methylisourea (107 g) and triethylamine (90 g) in anhydrous THF (800 ml) under nitrogen at -70° C. The resulting suspension is warmed to RT, filtered and the filtrate evaporated in vacuo. The residue is partitioned between methylene chloride and 0.5N aq. HCl. The organic layer is dried, filtered, and concentrated in vacuo affording the desired product as an oil.

후처리

  1. filtrationfiltered
  2. customthe filtrate evaporated in vacuo
  3. customThe residue is partitioned between methylene chloride and 0.5N aq. HCl
  4. customThe organic layer is dried
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-7893914eec8143aa87ab92f4bb98fbdd
출처 데이터셋
uspto-grants-1986_06
특허 번호
US04595683

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