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Hydrochloric Acid → Ethyl 2-[(2,2-dichloro-1-oxoethyl)-amino]-beta-oxo-alpha-[(2-thiazolylamino)-carbonyl]-3-(trifluoromethyl)-benzene-propanoate

HRID 1789217
ノート
印刷プレビュー

反応式

HRID 1789217 の反応式
[Cl:1][CH:2]([Cl:18])[C:3]1[O:8][C:7](=[O:9])[C:6]2[CH:10]=[CH:11][CH:12]=[C:13]([C:14]([F:17])([F:16])[F:15])[C:5]=2[N:4]=1.[S:19]1[CH:23]=[CH:22][N:21]=[C:20]1[NH:24][C:25](=[O:32])[CH2:26][C:27]([O:29][CH2:30][CH3:31])=[O:28].[OH-].[Na+].Cl>O.O1CCCC1>[Cl:1][CH:2]([Cl:18])[C:3]([NH:4][C:5]1[C:13]([C:14]([F:17])([F:16])[F:15])=[CH:12][CH:11]=[CH:10][C:6]=1[C:7](=[O:9])[CH:26]([C:25]([NH:24][C:20]1[S:19][CH:23]=[CH:22][N:21]=1)=[O:32])[C:27]([O:29][CH2:30][CH3:31])=[O:28])=[O:8]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 7339584Ethyl 3-oxo-3-(1,3-thiazol-2-ylamino)propanoateHCID 133813212-(Dichloromethyl)-8-(trifluoromethyl)-4H-3,1-benzoxazin-4-one

生成物 1

HCID 20188954Ethyl 2-[(2,2-dichloro-1-oxoethyl)-amino]-beta-oxo-alpha-[(2-thiazolylamino)-carbonyl]-3-(trifluoromethyl)-benzene-propanoate収率 98.9%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
20 °C

実験手順

At 20° C., 150 g of 2-dichloromethyl-8-trifluoromethyl-4H-3,1-benzoxazine-4-one, 120 g of ethyl 3-(2-thiazolylamino)-3-oxo-propanoate and 1.5 liters of tetrahydrofuran were mixed together and stirred for 30 minutes and then, while maintaining the temperature at 20° C., 40 g of sodium hydroxide in flakes were added thereto. After stirring the mixture at 20° C. for two hours, it was poured into a mixture of 4.5 liters of water and 150 ml of concentrated hydrochloric acid and the mixture was stirred at 0° to +5° C. for 30 minutes. The crystals formed were separated, rinsed with water and dried to obtain 255 g of ethyl 2-[(2,2-dichloro-1-oxoethyl)-amino]-β-oxo-α-[(2-thiazolylamino)-carbonyl]-3-(trifluoromethyl)-benzene-propanoate melting at 90° C.

後処理

  1. stirringAfter stirring the mixture at 20° C. for two hours
  2. stirringthe mixture was stirred at 0° to +5° C. for 30 minutes
  3. customThe crystals formed
  4. customwere separated
  5. washrinsed with water
  6. customdried

出典と根拠

ORDレコード
ord-6c40390b38bd4fa3b03a4392347326e9
出典データセット
uspto-grants-1987_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04687857

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート