Sodium Sulfate → HCID 89543564、化合物

HRID 922781ノート

反応式

HRID 922781 の反応式
[CH:1]1([CH:4]2[CH2:9][NH:8][C:7](=O)[CH2:6][S:5]2)[CH2:3][CH2:2]1.[H-].[H-].[H-].[H-].[Li+].[Al+3].[O-]S([O-])(=O)=O.[Na+].[Na+]>C1COCC1>[CH:1]1([CH:4]2[S:5][CH2:6][CH2:7][NH:8][CH2:9]2)[CH2:3][CH2:2]1

参加物

5

反応物 3

HCID 24436Sodium SulfateHCID 21226445Aluminium lithium hydrideHCID 89543728HCID 89543728、化合物

生成物 1

HCID 89543564HCID 89543564、化合物収率 75%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A solution of 6-cyclopropylthiomorpholin-3-one (4-13, 355 mg, 2.258 mmol) in THF (10 ml) was cooled to 0° C. To this was added 2M LAH (2.3 ml, 4.60 mmol) slowly. After the addition was complete the cooling bath was removed and the mixture allowed to warm to rt. After stirring overnight the mixture was cooled to 0° C. and slowly quenched with 2M NaOH until gas evolution had ceased and a fine white precipitate formed. Anhydrous Na2SO4 was added and the mixture stirred for 15 minutes. The slurry was filtered through a pad of Celite washing with THF and the filtrate concentrated to afford 2-cyclopropylthiomorpholine (4-14, 242 mg, 75%) as a pale yellow oil which was used in subsequent steps as is.

後処理

  1. additionAfter the addition
  2. customwas removed
  3. temperaturewas cooled to 0° C.
  4. customslowly quenched with 2M NaOH until gas evolution
  5. customa fine white precipitate formed
  6. stirringthe mixture stirred for 15 minutes
  7. filtrationThe slurry was filtered through a pad of Celite
  8. washwashing with THF
  9. concentrationthe filtrate concentrated

出典と根拠

ORDレコード
ord-06ed3f94c7d64b27827299239f0e3200
出典データセット
uspto-grants-2016_03
特許番号
US09278960B2

反応ノート

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