Triethylamine → 7-chloro-9-methyl-5-(N-ethylsulfonylamino)-2,3,4,5-tetrahydro-1-benzoxepine

HRID 2271082노트

반응식

HRID 2271082 반응식
[CH2:1]([S:3](Cl)(=[O:5])=[O:4])[CH3:2].[NH2:7][CH:8]1[C:14]2[CH:15]=[C:16]([Cl:20])[CH:17]=[C:18]([CH3:19])[C:13]=2[O:12][CH2:11][CH2:10][CH2:9]1.C(N(CC)CC)C>C1COCC1>[Cl:20][C:16]1[CH:17]=[C:18]([CH3:19])[C:13]2[O:12][CH2:11][CH2:10][CH2:9][CH:8]([NH:7][S:3]([CH2:1][CH3:2])(=[O:5])=[O:4])[C:14]=2[CH:15]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 11667Ethanesulfonyl chlorideHCID 223917895-Amino-7-chloro-9-methyl-2,3,4,5-tetrahydro-1-benzoxepine

생성물 1

HCID 223917937-chloro-9-methyl-5-(N-ethylsulfonylamino)-2,3,4,5-tetrahydro-1-benzoxepine수율 85.8%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

0.86 g of ethanesulfonyl chloride was added dropwise with ice-cooling to a solution of 1.3 g of 5-amino-7-chloro-9-methyl-2,3,4,5-tetrahydro-1-benzoxepine and 2.4 g of triethylamine in 30 ml of THF. The mixture was allowed to come to room temperature and was stirred overnight, and the solvent was distilled off in vacuo. After stirring the residue with water, the deposited product was filtered off with suction and dried in vacuo. 1.6 g of 7-chloro-9-methyl-5-(N-ethylsulfonylamino)-2,3,4,5-tetrahydro-1-benzoxepine were obtained, m.p. 144-145° C.

후처리

  1. customto come to room temperature
  2. distillationthe solvent was distilled off in vacuo
  3. stirringAfter stirring the residue with water
  4. filtrationthe deposited product was filtered off with suction
  5. customdried in vacuo

출처 및 근거

ORD 기록
ord-2395683f46e5417698c5c6252117a9e5
출처 데이터셋
uspto-grants-2001_12
특허 번호
US06333349B1

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