Trimethylboroxine → (3aS)-1-methyl-3,3-diphenyl-hexahydropyrrolo(1,2-c)(1,3,2)oxazaborole

HRID 1004491

反応式

HRID 1004491 の反応式
[C:1]1([C:7]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)([C@@H:9]2[CH2:13][CH2:12][CH2:11][NH:10]2)[OH:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:20][B:21]1OB(C)OB(C)O1>C1(C)C=CC=CC=1>[C:1]1([C:7]2([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[O:8][B:21]([CH3:20])[N:10]3[CH2:11][CH2:12][CH2:13][C@@H:9]23)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

参加物

4

反応物 2

HCID 574072TrimethylboroxineHCID 27248992-Pyrrolidinemethanol, alpha,alpha-diphenyl-, (S)-

生成物 1

HCID 2734713(3aS)-1-methyl-3,3-diphenyl-hexahydropyrrolo(1,2-c)(1,3,2)oxazaborole収率 100%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

Under argon stream, to a solution of (S)-α,α-diphenyl-2-pyrrolidine methanol (3 g, 11.8 mmol) in dry toluene (90 ml) was added trimethyl boroxine (1.13 ml, 8.0 mmol), followed by stirring for 1.5 hours. After the argon stream was stopped and the toluene (22.5 ml) was recovered under normal pressures on an oil bath at 140° C., dry toluene (22.5 ml) was added. Furthermore, after this recovery operation was repeated twice, the resultant product was concentrated under normal pressures, and subsequently under a reduced pressure, to thereby obtain the titled compound as a colorless crystalline.

後処理

  1. customthe toluene (22.5 ml) was recovered under normal pressures on an oil bath at 140° C.
  2. additiondry toluene (22.5 ml) was added
  3. concentrationthe resultant product was concentrated under normal pressures

出典と根拠

ORDレコード
ord-4a63ecdf7488425e96ba5e72240b0c99
出典データセット
uspto-grants-2000_04
特許番号
US06049009

関連ノート

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