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

Ethyl chloroformate → Tris(8-ethoxycarbonyl-2,2,6,6-tetramethylbenzo[1,2-d:4,5-d']-bis(1,3)dioxole-4-yl)methane

HRID 400280
노트
인쇄 미리보기

반응식

HRID 400280 반응식
[CH3:1][C:2]1([CH3:49])[O:6][C:5]2[C:7]([CH:16]([C:33]3[C:43]4[O:44][C:45]([CH3:48])([CH3:47])[O:46][C:42]=4[CH:41]=[C:35]4[O:36][C:37]([CH3:40])([CH3:39])[O:38][C:34]=34)[C:17]3[C:27]4[O:28][C:29]([CH3:32])([CH3:31])[O:30][C:26]=4[CH:25]=[C:19]4[O:20][C:21]([CH3:24])([CH3:23])[O:22][C:18]=34)=[C:8]3[O:12][C:11]([CH3:14])([CH3:13])[O:10][C:9]3=[CH:15][C:4]=2[O:3]1.[Li]CC[CH2:53][CH3:54].[CH2:55]([O:57][C:58](Cl)=[O:59])[CH3:56]>C1COCC1>[CH2:55]([O:57][C:58]([C:41]1[C:35]2[O:36][C:37]([CH3:40])([CH3:39])[O:38][C:34]=2[C:33]([CH:16]([C:17]2[C:18]3[O:22][C:21]([CH3:23])([CH3:24])[O:20][C:19]=3[C:25]([C:11]([O:12][CH2:53][CH3:54])=[O:10])=[C:26]3[O:30][C:29]([CH3:31])([CH3:32])[O:28][C:27]=23)[C:7]2[C:5]3[O:6][C:2]([CH3:49])([CH3:1])[O:3][C:4]=3[C:15]([C:2]([O:3][CH2:4][CH3:5])=[O:6])=[C:9]3[O:10][C:11]([CH3:13])([CH3:14])[O:12][C:8]=23)=[C:43]2[C:42]=1[O:46][C:45]([CH3:48])([CH3:47])[O:44]2)=[O:59])[CH3:56]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 10928Ethyl chloroformateHCID 67729115Tris(2,2,6,6-tetramethyl-benzo[1,2-d:4,5-d']bis(1,3)-dioxole-4-yl)methaneHCID 178418339Butyllithium

생성물 1

HCID 18943071Tris(8-ethoxycarbonyl-2,2,6,6-tetramethylbenzo[1,2-d:4,5-d']-bis(1,3)dioxole-4-yl)methane수율 45.9%

시약·촉매·용매 1

HCID 8028
Tetrahydrofuran
용매
2회

반응 조건

온도
-60 °C

실험 절차

Tris(2,2,6,6-tetramethylbenzo[1,2-d:4,5-d']-bis(1,3)dioxole-4-yl)methane (1.35 g, 2.0 mmol (Example 17)) was dissolved in dry THF (400 mL) under N2, and the temp was lowered to -40° C. and n-BuLi (4.86 mL, 12.2 mmol) was added and the temperature was allowed to rise gradually to 0° C. The mixture was cooled to -60° C., and a solution of ethylchloroformate (4.0, 36.7 mmol) in THF (50 mL) was added. The reaction mixture was left overnight and worked up as described under Example 20 above. The chromatography gave (0.41 g, 24%) of tris(8-ethoxycarbonyl-2,2,6,6-tetramethylbenzo[1,2-d:4,5-d']-bis(1,3)dioxole-4-yl)methane.

후처리

  1. customwas lowered to -40° C.
  2. customto rise gradually to 0° C

출처 및 근거

ORD 기록
ord-1597a8428c5a45598998ab6a074da8c8
출처 데이터셋
uspto-grants-1998_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05827501

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트