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Chloroacetyl chloride → (4R)-3-(Chloroacetyl)-1,3-thiazolidine-4-carboxamide

HRID 1015522
ノート
印刷プレビュー

反応式

HRID 1015522 の反応式
Cl.[S:2]1[CH2:6][C@@H:5]([C:7]([NH2:9])=[O:8])[NH:4][CH2:3]1.CCN(CC)CC.[Cl:17][CH2:18][C:19](Cl)=[O:20]>ClCCl>[Cl:17][CH2:18][C:19]([N:4]1[C@H:5]([C:7]([NH2:9])=[O:8])[CH2:6][S:2][CH2:3]1)=[O:20]
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

5

反応物 3

HCID 6577Chloroacetyl chlorideHCID 8471TriethylamineHCID 66879498HCID 66879498、化合物

生成物 1

HCID 45081035(4R)-3-(Chloroacetyl)-1,3-thiazolidine-4-carboxamide収率 99.7%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
0 °C

実験手順

To a stirred suspension of the hydrochloride salt obtained in step III (16.5 g, 0.1 mol) in dichloromethane (200 mL) cooled to 0° C. were added Et3N (41 mL, 0.3 mol) and chloroacetyl chloride (8.8 mL, 0.11 mol). The reaction mixture was slowly warmed to room temperature and stirred for 1 h. The reaction mass was filtered through a sintered funnel, the salt bed was washed with ether, and the filtrate was evaporated under vacuum to obtain the crude product (4R)-3-(chloroacetyl)-1,3-thiazolidine-4-carboxamide (20.8 g) as viscous liquid, which was used in the next step without further purification. m/z (M+1) 209; IR cm−1 3418, 2925, 1736, 1667, 1416, 1219, 771; 1H NMR (CDCl3) 300 MHz δ 6.60-6.30 (s (br), ½H), 6.0-5.65 (s (br), ½H), 5.02 (dd, J=3.6, 6.9 Hz, 0.8H), 4.88-4.75 (m, 0.4H), 4.70 (d, J=8.8 Hz, 0.8H), 4.62 (d, J=8.8 Hz, 0.8H), 4.51 (d, J=10.0 Hz, 0.2H), 4.16 (s, 1.6H), 4.11 (s, 0.4H), 3.56 (dd, J=3.4, 11.8 Hz, 0.8H), 3.44 (dd, J=4.7, 8.0 Hz, 0.4H), 3.15 (dd, J=7.1, 11.8 Hz, 0.8H), 1.28 (s, 1.6H), 1.25 (s, 7.4H).

後処理

  1. temperatureThe reaction mixture was slowly warmed to room temperature
  2. filtrationThe reaction mass was filtered through a sintered funnel
  3. washthe salt bed was washed with ether
  4. customthe filtrate was evaporated under vacuum

出典と根拠

ORDレコード
ord-78c51de537e741c787b8096a62ebcfb4
出典データセット
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07985759B2

反応ノート

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