Triethylamine → Tert-butyl (3R)-3-(methanesulfonyloxy)pyrrolidine-1-carboxylate

HRID 79303

反応式

HRID 79303 の反応式
[OH:1][C@@H:2]1[CH2:6][CH2:5][N:4]([C:7]([O:9][C:10]([CH3:13])([CH3:12])[CH3:11])=[O:8])[CH2:3]1.[CH3:14][S:15](Cl)(=[O:17])=[O:16].C(N(CC)CC)C>C(Cl)Cl>[CH3:14][S:15]([O:1][C@@H:2]1[CH2:6][CH2:5][N:4]([C:7]([O:9][C:10]([CH3:13])([CH3:12])[CH3:11])=[O:8])[CH2:3]1)(=[O:17])=[O:16]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 6544479tert-Butyl (3R)-3-hydroxypyrrolidine-1-carboxylate

生成物 1

HCID 10934372Tert-butyl (3R)-3-(methanesulfonyloxy)pyrrolidine-1-carboxylate収率 106.2%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To (R)-tert-butyl 3-hydroxypyrrolidine-1-carboxylate (87 mg, 0.465 mmol) in DCM (2 mL) at 0° C. was added methanesulfonyl chloride (58.5 mg, 0.511 mmol) and triethylamine (56.4 mg, 0.558 mmol). The cold bath was removed and the reaction was stirred for 30 minutes. The reaction was diluted with 5 mL DCM, washed with water and brine, dried (Na2SO4) and concentrated to give final product (131 mg).

後処理

  1. customThe cold bath was removed
  2. additionThe reaction was diluted with 5 mL DCM
  3. washwashed with water and brine
  4. dry with materialdried (Na2SO4)
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-3a359064b91246489d54f87d757c0d18
出典データセット
uspto-grants-2014_09
特許番号
US08841455B2

関連ノート

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