Triethylamine → HCID 20031878、化合物

HRID 231964ノート

反応式

HRID 231964 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-ebe2cbd99abe4feda08be550c1374de2
出典データセット
uspto-grants-1989_07
特許番号
US04849419

反応ノート

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