Diisopropyl Ether → (2Z)-2-[2-(dimethylaminomethylideneamino)-1,3-thiazol-4-yl]-2-methoxyiminoacetyl chloride;hydrochloride

HRID 266245

反応式

HRID 266245 の反応式
[Cl-:1].[CH3:2][N:3]([NH+]=C[Cl:7])[CH3:4].[NH2:8][C:9]1[S:10][CH:11]=[C:12](/[C:14](=[N:18]/[O:19][CH3:20])/[C:15]([OH:17])=O)[N:13]=1.[CH:21](OC(C)C)(C)C>O1CCCC1>[ClH:7].[CH3:2][N:3]([CH:4]=[N:8][C:9]1[S:10][CH:11]=[C:12](/[C:14](=[N:18]/[O:19][CH3:20])/[C:15]([Cl:1])=[O:17])[N:13]=1)[CH3:21]

参加物

5

反応物 3

HCID 7914Diisopropyl EtherHCID 5486924(alphaZ)-2-Amino-alpha-(methoxyimino)-4-thiazoleacetic acidHCID 86750850Dimethylaminochloromethyleneammonium chloride

生成物 1

HCID 140382097(2Z)-2-[2-(dimethylaminomethylideneamino)-1,3-thiazol-4-yl]-2-methoxyiminoacetyl chloride;hydrochloride収率 96.9%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
-12 °C

実験手順

Dimethylaminochloromethyleneammonium chloride (1.54 g, 12.0 mmol) was dissolved in 7 ml of tetrahydrofuran, followed by cooling to -12° C. Added to the solution were 1.10 g (5.5 mmol) of (Z)-2-(2-aminothiazol-4-yl)-2-methoxyiminoacetic acid and the resulting mixture was stirred for 40 minutes. Isopropyl ether (16 ml) was added to the reaction mixture, followed by stirring for 40 minutes. Deposited crystals were collected under a nitrogen gas stream, collected by filtration and then dried, whereby 1.65 g of the title compound were obtained (yield: 96.9%).

後処理

  1. additionAdded to the solution
  2. stirringby stirring for 40 minutes
  3. customDeposited crystals were collected under a nitrogen gas stream
  4. filtrationcollected by filtration
  5. customdried

出典と根拠

ORDレコード
ord-a2d5756d3e9f45d38aee089027d73d8e
出典データセット
uspto-grants-1997_07
特許番号
US05650518

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