Calcium Chloride → HCID 178488150、化合物

HRID 649144ノート

反応式

HRID 649144 の反応式
[Cl-].[Cl-].[Ca+2:3].[Na].[CH3:5][O:6][C:7]1[CH:28]=[CH:27][C:10]2[NH:11][C:12]([S:14]([CH2:16][C:17]3[C:22]([CH3:23])=[C:21]([O:24][CH3:25])[C:20]([CH3:26])=[CH:19][N:18]=3)=[O:15])=[N:13][C:9]=2[CH:8]=1>O>[CH3:26][C:20]1[CH:19]=[N:18][C:17]([CH2:16][S+:14]([O-:15])[C:12]2[NH:11][C:10]3[CH:27]=[CH:28][C:7]([O:6][CH3:5])=[CH:8][C:9]=3[N:13]=2)=[C:22]([CH3:23])[C:21]=1[O:24][CH3:25].[Ca:3]

参加物

4

反応物 2

HCID 5284359Calcium ChlorideHCID 178488156HCID 178488156、化合物

生成物 1

HCID 178488150HCID 178488150、化合物収率 80%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

Anhydrous CaCl2 (17.9 g, 0.161 mol) dissolved in deionized water (200 ml) was added dropwise under viogorous stirring to a solution of omeprazole sodium salt (125 g, 0.340 mole) in deionized water (1250 ml) and then stirring was continued for 1 h at room temperature. The precipitate was centrifuged down and washed with deionized water until no Cl- was detectable (AgNO3). After drying in the air and grinding, the crystals were dried in vacuum at 40° for 20 h yielding omeprazole calcium salt dihydrate (104 mg, 80%), mp 182°-184° C., NMR: δ(CDCl3 1 drop of DMSO-d6) 2.0(s, 3H), 2.15(s, 3H), 3.6(s, 3H), 3.7(s, 3H), 4.5(s, 2H), 6.7(dd, 1H), 7.1(d, 1H), 7.6(d, 1H, 8.15(s, 1H).

後処理

  1. additionwas added dropwise
  2. washwashed with deionized water until no Cl-
  3. customAfter drying in the air
  4. customgrinding
  5. customthe crystals were dried in vacuum at 40° for 20 h

出典と根拠

ORDレコード
ord-3494ae02c29348f49a2ca553da34489a
出典データセット
uspto-grants-1988_04
特許番号
US04738974

反応ノート

読み込み中…