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

Tetrahydrofuran → HCID 136414663, 화합물

HRID 645304
노트
인쇄 미리보기

반응식

HRID 645304 반응식
[Cl:1][C:2]1[CH:3]=[C:4]([C:9]([C:23]([F:26])([F:25])[F:24])=[CH:10][C:11]([C:13]2[CH:21]=[CH:20][C:16]([C:17]([NH2:19])=[O:18])=[C:15]([CH3:22])[CH:14]=2)=[O:12])[CH:5]=[C:6]([Cl:8])[CH:7]=1.CO[CH:29](OC)[N:30](C)C.[O:35]1[CH2:39]CCC1>>[Cl:1][C:2]1[CH:3]=[C:4]([C:9]([C:23]([F:26])([F:24])[F:25])=[CH:10][C:11]([C:13]2[CH:21]=[CH:20][C:16]([C:17]([NH:19][CH:29]=[N:30][O:35][CH3:39])=[O:18])=[C:15]([CH3:22])[CH:14]=2)=[O:12])[CH:5]=[C:6]([Cl:8])[CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 8028TetrahydrofuranHCID 78373Dimethylformamide dimethyl acetalHCID 66738433HCID 66738433, 화합물

생성물 1

HCID 136414663HCID 136414663, 화합물

실험 절차

To a solution of 0.18 g of 4-(3-(3,5-dichlorophenyl)-4,4,4-trifluoro-2-butenoyl)-2-methylbenzoic acid amide representing mixed geometrical isomers (isomeric ratio of 10:1) that was synthesized according to Synthetic Example 9 in 3 mL of tetrahydrofuran, 0.11 g of N,N-dimethylformamide dimethyl acetal was added and the mixture was stirred for 2 hours at room temperature. After that, the solvent was distilled off under reduced pressure, the resulting residue was dissolved in 3 mL of tetrahydrofuran, and a solution of 45 mg of methoxyamine hydrochloride in 1 mL of water was dripped in at room temperature. After the mixture was stirred for 1.5 hours, whereinto ethyl acetate was added, an organic layer was washed twice with water and then dehydrated and dried with saturated saline followed by anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. By washing the resulting solid with a mixed solvent of diisopropylether and acetonitrile, 60 mg of aimed product was obtained as pale yellow solid.

후처리

  1. customwas synthesized
  2. distillationAfter that, the solvent was distilled off under reduced pressure
  3. dissolutionthe resulting residue was dissolved in 3 mL of tetrahydrofuran
  4. customwas dripped in at room temperature
  5. stirringAfter the mixture was stirred for 1.5 hours, whereinto ethyl acetate
  6. additionwas added
  7. washan organic layer was washed twice with water
  8. customdried with saturated saline
  9. distillationthe solvent was distilled off under reduced pressure
  10. washBy washing the resulting solid with a mixed solvent of diisopropylether and acetonitrile

출처 및 근거

ORD 기록
ord-96dd84b3b3fb4db0aab851af7f3a47e3
출처 데이터셋
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07700808B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트