Trifluoroacetic acid → HCID 21957075、化合物

HRID 2214272ノート

反応式

HRID 2214272 の反応式
C([O:5][C:6](=[O:51])[CH:7]([NH:16][C:17](=[O:50])[CH:18]([CH2:42][C:43]([O:45]C(C)(C)C)=[O:44])[CH2:19][CH2:20][CH2:21][S:22]C(C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[CH2:8][C:9]([O:11]C(C)(C)C)=[O:10])(C)(C)C.C(O)(C(F)(F)F)=O.C(S)(S)C.C([SiH](C(C)C)C(C)C)(C)C>C(Cl)Cl>[C:43]([CH2:42][CH:18]([CH2:19][CH2:20][CH2:21][SH:22])[C:17]([NH:16][CH:7]([CH2:8][C:9]([OH:11])=[O:10])[C:6]([OH:51])=[O:5])=[O:50])([OH:45])=[O:44]

参加物

6

反応物 4

HCID 6422Trifluoroacetic acidHCID 336451,1-EthanedithiolHCID 138754Silane, tris(1-methylethyl)-HCID 69211675HCID 69211675、化合物

生成物 1

HCID 21957075HCID 21957075、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To the protected thiolate of Example 119 in CH2Cl2 (1 mL) was added at 0° C. a solution of 60% TFA in CH2Cl2, containing 2% of ethanedithiol. Triisopropyl silane (1%) was then added and the reaction mixture was stirred at room temperature for 1 hour after which it was first concentrated using a stream of argon and then under vacuum. The obtained white solid was washed several times with a mixture of diethyl ether/hexanes (3:1). The obtained white solid was purified by semi-preparative HPLC to provide the desired compound.

後処理

  1. concentrationwas first concentrated
  2. washThe obtained white solid was washed several times
  3. additionwith a mixture of diethyl ether/hexanes (3:1)
  4. customThe obtained white solid was purified by semi-preparative HPLC

出典と根拠

ORDレコード
ord-6c5f9f5741bb44f09185701db5b81c74
出典データセット
uspto-grants-2006_09
特許番号
US07105539B2

反応ノート

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