Hydrochloric Acid → HCID 46945559、化合物

HRID 2370600ノート

反応式

HRID 2370600 の反応式
Cl.[CH3:2][C:3]1([CH3:49])[C:7](=[O:8])[N:6]([C:9]2[CH:14]=[CH:13][C:12]([NH:15][S:16]([NH:19]C(=O)OC(C)(C)C)(=[O:18])=[O:17])=[C:11]([CH3:27])[CH:10]=2)[C:5](=[O:28])[N:4]1[CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][S:38][CH2:39][CH2:40][CH2:41][C:42]([F:48])([F:47])[C:43]([F:46])([F:45])[F:44].C(Cl)Cl.CCOC(C)=O>C(OCC)C>[CH3:2][C:3]1([CH3:49])[C:7](=[O:8])[N:6]([C:9]2[CH:14]=[CH:13][C:12]([NH:15][S:16]([NH2:19])(=[O:18])=[O:17])=[C:11]([CH3:27])[CH:10]=2)[C:5](=[O:28])[N:4]1[CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH2:37][S:38][CH2:39][CH2:40][CH2:41][C:42]([F:48])([F:47])[C:43]([F:44])([F:45])[F:46]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 21226138Dichloromethane ethylacetateHCID 123569579HCID 123569579、化合物

生成物 1

HCID 46945559HCID 46945559、化合物収率 76%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

反応条件

温度
0 °C

実験手順

A solution of HCl in ethyl ether (2N, 3 ml) is added in 31-ml portions to a solution of Example 29 (250 mg, 0.36 mmole) in a CH2Cl2/AcOEt mixture (5 ml/3 ml) cooled down to 0° C., and the mixture is stirred for 60 hours at 23° C. The volatiles are evaporated off under vacuum and the residue is taken up in a CH2Cl2 (50 ml) and NaHCO3 (50 ml) mixture. After stirring and decantation, the organic phase is washed with water (50 ml) followed by salt water. After drying over Na2SO4, filtration and concentration to dryness, the residue is purified on a silica column (Heptane/AcOEt:10/0 to 1/1). The expected product is obtained in the form of a white solid with a yield of 76%. Melting point: 102-104° C.

後処理

  1. customThe volatiles are evaporated off under vacuum
  2. stirringAfter stirring
  3. washdecantation, the organic phase is washed with water (50 ml)
  4. dry with materialAfter drying over Na2SO4, filtration and concentration to dryness
  5. customthe residue is purified on a silica column (Heptane/AcOEt:10/0 to 1/1)

出典と根拠

ORDレコード
ord-77e5e8f591b04f6985924204104dd802
出典データセット
uspto-grants-2014_04
特許番号
US08710091B2

反応ノート

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