Hydrochloric Acid → HCID 178477875, 화합물

HRID 232850노트

반응식

HRID 232850 반응식
C[Sn]([N:5]=[N+:6]=[N-:7])(C)C.[Cl:8][C:9]1[CH:18]=[C:17]2[C:12]([CH:13]=[CH:14][C:15]([CH2:19][O:20][C:21]3[CH:40]=[CH:39][C:24]4[O:25][CH2:26][C:27]5[CH:38]=[CH:37][CH:36]=[CH:35][C:28]=5[CH:29]([S:30][CH2:31][CH2:32][C:33]#[N:34])[C:23]=4[CH:22]=3)=[N:16]2)=[CH:11][CH:10]=1.Cl.[OH-].[Na+]>C1(C)C(C)=CC=CC=1>[Cl:8][C:9]1[CH:18]=[C:17]2[C:12]([CH:13]=[CH:14][C:15]([CH2:19][O:20][C:21]3[CH:40]=[CH:39][C:24]4[O:25][CH2:26][C:27]5[CH:38]=[CH:37][CH:36]=[CH:35][C:28]=5[CH:29]([S:30][CH2:31][CH2:32][C:33]5[NH:34][N:7]=[N:6][N:5]=5)[C:23]=4[CH:22]=3)=[N:16]2)=[CH:11][CH:10]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 5104973Azido(trimethyl)stannaneHCID 233591442-(7-Chloroquinolin-2-yl)methoxy-11-(2-cyanoethylthio)-6,11-dihydrodibenz[b,e]oxepine

생성물 1

HCID 178477875HCID 178477875, 화합물수율 4.6%

시약·촉매·용매 1

HCID 7237O-Xylene용매

실험 절차

1.25 g of trimethyltin azide was added to 1.4 g of 2-(7-chloroquinolin-2-yl)methoxy-11-(2-cyanoethylthio)-6,11-dihydrodibenz[b,e]oxepine dissolved in 40 ml of xylene and the mixture was refluxed under heating for 8.5 hours. After cooling, 1.5 ml of conc. hydrochloric acid was added to the mixture and the mixture was stirred at room temperature for 15 minutes and then adjusted to about pH 4 with a 1N-sodium hydroxide aqueous solution. Crystals precipitated were applied to silica gel column chromatography to obtain 70 mg of the title compound as light orange powder.

후처리

  1. temperaturethe mixture was refluxed
  2. temperatureunder heating for 8.5 hours
  3. temperatureAfter cooling
  4. customCrystals precipitated

출처 및 근거

ORD 기록
ord-9c0a64eb273e4564936a45efb716099b
출처 데이터셋
uspto-grants-1997_01
특허 번호
US05591752

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