홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

1,2-Dichloroethane → HCID 86758351, 화합물

HRID 2229221
노트
인쇄 미리보기

반응식

HRID 2229221 반응식
[CH2:1]([O:3][P:4]([C:9]1[C:10](=[O:21])[NH:11][C:12]2[C:17]([CH:18]=1)=[CH:16][C:15]([NH2:19])=[C:14]([Cl:20])[CH:13]=2)(=[O:8])[O:5][CH2:6][CH3:7])[CH3:2].CO[CH:24]1[CH2:28][CH2:27][CH:26](OC)O1.C(O)(=O)C.ClCCCl>O.C(Cl)Cl.CO>[CH2:1]([O:3][P:4]([C:9]1[C:10](=[O:21])[NH:11][C:12]2[C:17]([CH:18]=1)=[CH:16][C:15]([N:19]1[CH:24]=[CH:28][CH:27]=[CH:26]1)=[C:14]([Cl:20])[CH:13]=2)(=[O:8])[O:5][CH2:6][CH3:7])[CH3:2]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 111,2-DichloroethaneHCID 176Acetic AcidHCID 790982,5-Dimethoxytetrahydrofuran2회HCID 15511753HCID 15511753, 화합물

생성물 1

HCID 86758351HCID 86758351, 화합물

시약·촉매·용매 2

HCID 962Water용매
HCID 21226129
Dichloromethane methanol
용매

반응 조건

온도
75 °C

실험 절차

A biphasic suspension of 2.43 g (7.35 mmol) of the compound obtained in Step D of Example 1 and 1.33 ml (10.29 mmol) of 2,5-dimethoxytetrahydrofuran in a mixture of 24 ml of distilled water, 12 ml of acetic acid and 36 ml of 1,2-dichloroethane is stirred vigorously at 75° C. for 60 minutes. In TLC (CH2Cl2/MeOH 9:1), a small amount of starting material is still observed. 0.2 eq. of 2,5-dimethoxytetrahydrofuran (2.06 mmol, 0.26 ml) is added, and heating is maintained for 30 minutes. The mixture is left to return to room temperature and extraction is carried out with CH2Cl2. The organic phase is washed 4 times with water and then with a saturated NaCl solution. Drying is carried out over MgSO4, followed by evaporation and chromatography of the resulting oil over 200 g of Merck 7734 silica whilst eluting with a mixture of CH2Cl2/MeOH 95:5. An oil corresponding to the title product is obtained, which is crystallised from isopropyl ether.

후처리

  1. temperatureheating
  2. temperatureis maintained for 30 minutes
  3. waitThe mixture is left
  4. customto return to room temperature
  5. extractionextraction
  6. washThe organic phase is washed 4 times with water
  7. customDrying
  8. customfollowed by evaporation and chromatography of the resulting oil over 200 g of Merck 7734 silica
  9. washwhilst eluting with a mixture of CH2Cl2/MeOH 95:5

출처 및 근거

ORD 기록
ord-110df0efd9fd49ad8c8f6841ba6f8c03
출처 데이터셋
uspto-grants-2002_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06420386B1

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트