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HRID1978788

反应详情

EQUATION

反应方程式

HRID 1978788 的结构方程式

REACTANTS

反应物

2
结构：O=S(=O)(O)c1ccccc1
HCID7371

Benzenesulfonic acid

C6H6O3S

结构：CCCOCCOc1ccc(-c2ccc3c(c2)C=C(C(=O)Nc2ccc(CN(C)C4CCOCC4)cc2)CCS3(=O)=O)cc1
HCID3009396

未命名化合物

PRODUCTS

生成物

1
结构：CCCOCCOc1ccc(-c2ccc3c(c2)C=C(C(=O)Nc2ccc(CN(C)C4CCOCC4)cc2)CCS3(=O)=O)cc1.O=S(=O)(O)c1ccccc1
HCID21995841

未命名化合物

收率 86.2%

AUXILIARIES

试剂、催化剂与溶剂

1
结构：C1CCOC1
溶剂HCID8028

Tetrahydrofuran

C4H8O

PROCEDURE

实验过程

To a solution of N-[4-[N-methyl-N-(tetrahydropyran-4-yl)aminomethyl]phenyl]-7-[4-(2-propoxyethoxy)phenyl]-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxamide (1.10 g) in THF (40 ml) was added at room temperature benzenesulfonic acid (313 mg), and the mixture was stirred for 1 hour and concentrated under reduced pressure. To the residue was added 2-propanol, and the mixture was concentrated under reduced pressure. The residue was crystallized from 2-propanol to give crude crystals, which were recrystallized from 2-propanol to give colorless crystals of N-[4-[N-methyl-N-(tetrahydropyran-4-yl)aminomethyl]phenyl]-7-[4-(2-propoxyethoxy)phenyl]-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxamide benzenesulfonate (Compound 147) (1.19 g).

WORKUP

后处理

  1. concentrationconcentrated under reduced pressure
  2. additionTo the residue was added 2-propanol
  3. concentrationthe mixture was concentrated under reduced pressure
  4. customThe residue was crystallized from 2-propanol
  5. customto give crude crystals, which
  6. customwere recrystallized from 2-propanol