HCID 18712863, 화합물 → HCID 53914541, 화합물

HRID 392516노트

반응식

HRID 392516 반응식
CC([C@:5]1([C:31]([N:33]2[CH2:38][CH2:37][CH:36]([CH2:39][CH2:40][CH2:41][N:42]3[CH:46]=[CH:45][N:44]=[CH:43]3)[CH2:35][CH2:34]2)=[O:32])[CH2:10][N:9](C2C3=NC=C(Br)C=C3CCC3C=C(Cl)C=CC2=3)[CH2:8][CH2:7][N:6]1C([O-])=O)(C)C>ClCCl>[N:42]1([CH2:41][CH2:40][CH2:39][CH:36]2[CH2:37][CH2:38][N:33]([C:31]([C@H:5]3[CH2:10][NH:9][CH2:8][CH2:7][NH:6]3)=[O:32])[CH2:34][CH2:35]2)[CH:46]=[CH:45][N:44]=[CH:43]1

참가 물질

3

반응물 1

HCID 18712863HCID 18712863, 화합물

생성물 1

HCID 53914541HCID 53914541, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A solution of 3-peroxybenzoic acid (25 g, 102.59 mmol, 2.5 eq.) in anhydrous dichloromethane (250 mL) was added dropwise over a period of one hour to a stirred solution of 8-chloro-4-aza-10,11-dihydro-5H-dibenzo[a,d]cyclohepten-5-one 1 (10 g, 41.04 mmol, 1.0 eq.) in anhydrous dichloromethane (100 mL) at 0° C. under a nitrogen atmosphere. The solution was slowly (3 h) warmed to room temperature and stirred for another 12 h. The solution was extracted with 1 M aqueous sodium hydroxide solution (5×100 mL), washed with brine (2×100 mL), dried over Na2SO4, filtered, and concentrated under house vacuum at 30° C. to give 2 as a canary-yellow solid. The title compound 2 was used directly without further attempts at purification.

후처리

  1. custom(3 h)
  2. extractionThe solution was extracted with 1 M aqueous sodium hydroxide solution (5×100 mL)
  3. washwashed with brine (2×100 mL)
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated under house vacuum at 30° C.

출처 및 근거

ORD 기록
ord-8da3eb69304649da9fc3cbd0f2043d86
출처 데이터셋
uspto-grants-2004_10
특허 번호
US06800636B2

반응 노트

불러오는 중…