HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → 2-[Bis-(2-chloroethyl)amino]-4-chloro-6-methyl-10,10-dioxo-10,11-dihydro-5-oxa-10lambda*6*-thia-dibenzo[a,d]-cycloheptene-8-carboxylic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 2-[Bis-(2-chloro-ethyl)-amino]-4-chloro-6-methyl-10,10-dioxo-10,11-dihydro-5-oxa-10lambda*6*-thia-dibenzo[a,d]cycloheptene-8-carboxylic acid methyl ester | HCID 11526072 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 2-[Bis-(2-chloroethyl)amino]-4-chloro-6-methyl-10,10-dioxo-10,11-dihydro-5-oxa-10lambda*6*-thia-dibenzo[a,d]-cycloheptene-8-carboxylic acid | HCID 131728474 | — |
Reaction Steps
Aqueous sodium hydroxide (0.78 g, 19.6 mmol in 45 mL water) was added to a solution of Example 102 (3.21 g, 6.53 mmol) in tetrahydrofuran (45 mL). It was stirred for 3 h, partially concentrated, treated with dil. HCl to pH 7, filtered, washed with water and dried to obtain the title compound as a white solid. Yield: 3.01 g (97%). 1H NMR (CDCl3+DMSO-d6): δ 2.40 (s, 3H, CH3), 3.4 (t, 4H, 2CH2), 3.5 (t, 4H, 2CH2), 4.5 (s, 2H, CH2), 6.4 (d, 1H, Ar), 6.5 (d, 1H, Ar), 7.7 (d, 1H, Ar), 8.1 (d, 1H, Ar); MS: m/e (CI+) 478 (M+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07834001B2 |
| Source dataset | uspto-grants-2010_11 |
| ORD ID | ord-d8424e17c0ae4b2fa697ca1e23e8854b |
| Source note | uspto-grants-2010_11 |