Hydrochloric Acid → HCID 22386569, 화합물

HRID 1072481

반응식

HRID 1072481 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([NH2:24])[CH:5]=[C:6]([Cl:23])[C:7]=1[C:8]([C:11]1[N:15]=[C:14]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[CH3:22])[O:13][N:12]=1)([CH3:10])[CH3:9].Cl.[N:26]([O-])=O.[Na+].C([O-])(=O)C.[Na+].[CH2:35]([O:37][C:38](=[O:51])[NH:39][C:40](=[O:50])[CH2:41][C:42]([NH:44][C:45](=[O:49])[O:46][CH2:47][CH3:48])=[O:43])[CH3:36]>C(O)(=O)C.O>[Cl:1][C:2]1[CH:3]=[C:4]([NH:24][N:26]=[C:41]([C:42]([NH:44][C:45](=[O:49])[O:46][CH2:47][CH3:48])=[O:43])[C:40]([NH:39][C:38](=[O:51])[O:37][CH2:35][CH3:36])=[O:50])[CH:5]=[C:6]([Cl:23])[C:7]=1[C:8]([C:11]1[N:15]=[C:14]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[CH3:22])[O:13][N:12]=1)([CH3:10])[CH3:9]

참가 물질

8

반응물 5

HCID 313Hydrochloric AcidHCID 154305Carbamic acid, (1,3-dioxo-1,3-propanediyl)bis-, diethyl esterHCID 517045Sodium AcetateHCID 22386562HCID 22386562, 화합물HCID 23668193Sodium Nitrite

생성물 1

HCID 22386569HCID 22386569, 화합물

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 962Water용매2회

반응 조건

온도
0 °C

실험 절차

A solution of intermediate (19) (0.0302 mole) and concentrated HCl (0.0906 mole) in acetic acid (100 ml) was stirred at 0° C. A solution of NaNO2 (0.032 mole) in water (10 ml) was added dropwise at 0° C. The reaction mixture was stirred for 1 hour at 0° C. A powdered mixture of sodium acetate (0.0906 mole) and diethyl(1,3-dioxo-1,3-propanediyl)biscarbamate (0.0332 mole) was added portionwise. The mixture was allowed to warm to RT and stirred for 1 hour. Water was added and this mixture was extracted with CH2Cl2. The separated organic layer was dried, filtered and the solvent evaporated, yielding diethyl N,N′-[2-[[3,5-dichloro-4-[1-[5-(2-methylphenyl)-1,2,4-oxadiazol-3-yl]-1-methylethyl]phenyl]hydrazono]-1,3-dioxo-1,3-propanediyl]dicarbamate (intermediate 20).

후처리

  1. additionwas added portionwise
  2. temperatureto warm to RT
  3. stirringstirred for 1 hour
  4. extractionthis mixture was extracted with CH2Cl2
  5. customThe separated organic layer was dried
  6. filtrationfiltered
  7. customthe solvent evaporated

출처 및 근거

ORD 기록
ord-d4518b950bac4db98bb4394c28151e1f
출처 데이터셋
uspto-grants-2005_06
특허 번호
US06911444B2

연결된 노트

불러오는 중…