Triethylamine → HCID 20031878、化合物

HRID 2291293ノート

反応式

HRID 2291293 の反応式
[C:1]([Cl:4])(Cl)=[S:2].[OH:5][C:6]1[CH:7]=[C:8]([CH:29]=[CH:30][CH:31]=1)[C:9]([O:11][Si:12]([C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)([C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)[C:13]([CH3:16])([CH3:15])[CH3:14])=[O:10].C(N(CC)CC)C>C(OCC)C>[Cl:4][C:1]([O:5][C:6]1[CH:7]=[C:8]([CH:29]=[CH:30][CH:31]=1)[C:9]([O:11][Si:12]([C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)([C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)[C:13]([CH3:16])([CH3:14])[CH3:15])=[O:10])=[S:2]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 10040ThiophosgeneHCID 54284754HCID 54284754、化合物

生成物 1

HCID 20031878HCID 20031878、化合物

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒2 回

反応条件

温度
-78 °C

実験手順

To a stirred solution of 130 ml of thiophosgene in 250 ml of dry diethyl ether at -78° C. was added dropwise a mixture of 72 g of diphenyl- (2-methylprop-2-yl)silyl 3-hydroxybenzoate and 29 ml of triethylamine in 200 ml of dry diethyl ether. The mixture was stirred at -78° C. for 30 minutes, at room temperature for 120 minutes, and then partitioned between diethyl ether and water. The organic layer was washed with cold water and with brine, and was dried over anhydrous calcium chloride. Evaporation in vacuo, and repeated addition of dry diethyl ether and re-evaporation in vacuo afforded 86.5 g of the title compound as a viscous orange oil.

後処理

  1. custompartitioned between diethyl ether and water
  2. washThe organic layer was washed with cold water and with brine
  3. dry with materialwas dried over anhydrous calcium chloride
  4. customEvaporation in vacuo
  5. additionaddition of dry diethyl ether and re-evaporation in vacuo

出典と根拠

ORDレコード
ord-89028ea92ee2488eb6c9d0a867eb72f1
出典データセット
uspto-grants-1989_01
特許番号
US04795748

反応ノート

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