Sodium Iodide → HCID 54296994、化合物

HRID 1904148ノート

反応式

HRID 1904148 の反応式
Br[CH2:2][CH2:3][O:4][N:5]=[C:6]([C:12]1[N:13]=[C:14]([NH:17][C:18]([C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)([C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)[C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[S:15][CH:16]=1)[C:7]([O:9][CH2:10][CH3:11])=[O:8].[I-:37].[Na+]>C(C(C)=O)C>[I:37][CH2:2][CH2:3][O:4][N:5]=[C:6]([C:12]1[N:13]=[C:14]([NH:17][C:18]([C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)([C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)[C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[S:15][CH:16]=1)[C:7]([O:9][CH2:10][CH3:11])=[O:8]

参加物

4

反応物 2

HCID 5238Sodium IodideHCID 53679114Ethyl 2-(bromoethoxyimino)-2-(2-tritylamino-4-thiazolyl)-acetate

生成物 1

HCID 54296994HCID 54296994、化合物

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

実験手順

A mixture of 6 g of the syn isomer of ethyl 2-(2-bromoethoxyimino)-2-(2-tritylamino-4-thiazolyl)-acetate, 60 ml of methyl ethyl ketone and 2.141 g of sodium iodide was refluxed for 70 minutes and was then evaporated to dryness under reduced pressure. The residue was taken up in 120 ml of methylene chloride and the solution was washed 5 times with 40 ml of water. Each of the wash waters were reextracted with 2 ml of methylene chloride and the combined organic phase were dried and evaporated to dryness. The resin residue was added to ether and the solution was evaporated to dryness under reduced pressure to obtain 6.22 g of the syn isomer of ethyl 2-(2-iodoethoxyimino)-2-(2-tritylamino-4-thiazolyl)acetate melting at 110° C.

後処理

  1. temperaturewas refluxed for 70 minutes
  2. customwas then evaporated to dryness under reduced pressure
  3. washthe solution was washed 5 times with 40 ml of water
  4. customthe combined organic phase were dried
  5. customevaporated to dryness
  6. additionThe resin residue was added to ether
  7. customthe solution was evaporated to dryness under reduced pressure

出典と根拠

ORDレコード
ord-5cf8791f3126413d8f4e68d23f7cdfaf
出典データセット
uspto-grants-1984_03
特許番号
US04439433

反応ノート

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