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

Diisopropylethylamine → HCID 22644655, 화합물

HRID 2414310
노트
인쇄 미리보기

반응식

HRID 2414310 반응식
[Cl:1]C(Cl)(O[C:5](=[O:11])[O:6][C:7](Cl)(Cl)Cl)Cl.[Cl:13][C:14]1[CH:15]=[CH:16][C:17](CO)=[C:18]([NH:20][CH:21]2[CH2:26][CH2:25][N:24](C(OC(C)(C)C)=O)[CH2:23][CH2:22]2)[CH:19]=1.C(N(CC)C(C)C)(C)C>O1CCCC1>[ClH:1].[Cl:13][C:14]1[CH:15]=[CH:16][C:17]2[CH2:7][O:6][C:5](=[O:11])[N:20]([CH:21]3[CH2:26][CH2:25][NH:24][CH2:23][CH2:22]3)[C:18]=2[CH:19]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 81531DiisopropylethylamineHCID 94429TriphosgeneHCID 22644619HCID 22644619, 화합물

생성물 1

HCID 22644655HCID 22644655, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Triphosgene (1.6 g) was added to a stirred solution of the product from step (i) (5 g), N,N-diisopropylethylamine (5.2 ml) in tetrahydrofuran (50 ml) at 0° C. The mixture was stirred at room temperature for 16 h, the precipitate filtered and the filtrate evaporated under reduced pressure. Purification was by chromatography eluting with 20% ethyl acetate/toluene. The product was dissolved in dichloromethane then a solution of hydrogen chloride in 1,4-dioxane added. After 2 h the solvent was removed under reduced pressure to yield a solid. Used directly.

후처리

  1. filtrationthe precipitate filtered
  2. customthe filtrate evaporated under reduced pressure
  3. customPurification
  4. washeluting with 20% ethyl acetate/toluene
  5. dissolutionThe product was dissolved in dichloromethane
  6. additiona solution of hydrogen chloride in 1,4-dioxane added
  7. customAfter 2 h the solvent was removed under reduced pressure
  8. customto yield a solid

출처 및 근거

ORD 기록
ord-7ff984da44b649cdb086c1bb34d59d0d
출처 데이터셋
uspto-grants-2004_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06812226B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트