Dichloromethane → HCID 19989845, 화합물

HRID 973419

반응식

HRID 973419 반응식
[CH3:1][N:2]1[CH2:6][CH2:5][CH:4]([C:7]2[NH:11][C:10]3[CH:12]=[CH:13][CH:14]=[CH:15][C:9]=3[N:8]=2)[CH2:3]1.C(Cl)(Cl)=[O:17].C1(C)C=CC=CC=1.C(N(CC)CC)C.[CH2:34]([Cl:36])Cl>>[Cl:36][CH2:34][CH2:5][CH:4]1[C:7]2=[N:11][C:10]3[CH:12]=[CH:13][CH:14]=[CH:15][C:9]=3[N:8]2[C:1](=[O:17])[N:2]([CH3:6])[CH2:3]1

참가 물질

5

반응물 4

HCID 6344Dichloromethane2회HCID 8471TriethylamineHCID 19083224Phosgen tolueneHCID 19989862HCID 19989862, 화합물

생성물 1

HCID 19989845HCID 19989845, 화합물

실험 절차

A solution of 4 g (0.02 mol) of 2-(1-methyl-3-pyrrolidinyl)-1H-benzimidazole in 100 mL of CH2Cl2 was added dropwise to a solution of 12.5 (0.025 mol) of 20% phosgene/toluene in 30 mL of CH2Cl2. The solution was stirred for 2 h, and 10 g (0.1 mol) of triethylamine was added dropwise. Stirring was continued for 2 h and the solution was extracted with dilute NaOH. The organic layer was dried (Na2SO4) and concentrated. The residue was crystallized twice from isopropyl ether. Yield 1.5 g (28%), mp 88°-91° C.

후처리

  1. stirringStirring
  2. waitwas continued for 2 h
  3. extractionthe solution was extracted with dilute NaOH
  4. dry with materialThe organic layer was dried (Na2SO4)
  5. concentrationconcentrated
  6. customThe residue was crystallized twice from isopropyl ether

출처 및 근거

ORD 기록
ord-27f19568d9bd4b42a0e6cf1e47ac43b7
출처 데이터셋
uspto-grants-1991_11
특허 번호
US05063228

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