Morpholine → Toluene-4-thiosulfonic acid S-(3-morpholin-4-yl-propyl)ester

HRID 707675ノート

反応式

HRID 707675 の反応式
Cl[CH2:2][CH2:3][CH2:4][S:5][S:6]([C:9]1[CH:14]=[CH:13][C:12]([CH3:15])=[CH:11][CH:10]=1)(=[O:8])=[O:7].[NH:16]1[CH2:21][CH2:20][O:19][CH2:18][CH2:17]1.C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[N:16]1([CH2:2][CH2:3][CH2:4][S:5][S:6]([C:9]2[CH:14]=[CH:13][C:12]([CH3:15])=[CH:11][CH:10]=2)(=[O:8])=[O:7])[CH2:21][CH2:20][O:19][CH2:18][CH2:17]1

参加物

5

反応物 3

HCID 8083MorpholineHCID 11430Potassium CarbonateHCID 67607671Toluene-4-thiosulfonic acid S-(3-chloropropyl)ester

生成物 1

HCID 67605844Toluene-4-thiosulfonic acid S-(3-morpholin-4-yl-propyl)ester

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

Toluene-4-thiosulfonic acid S-(3-chloro-propyl) ester (61.7 g, 233 mmol, 1.00 eq.), morpholine (22.2 g, 255 mmol, 1.09 eq.) and potassium carbonate (33.8 g, 240 mmol, 1.06 eq.) were stirred together in acetonitrile (1 L) for 64 hours at 50° C. The mixture was concentrated, then partitioned between ethyl acetate and water. The organic solution was washed with water (2×), dried using MgSO4, and concentrated to produce a light yellow oil weighing 61.5 g (84%).

後処理

  1. concentrationThe mixture was concentrated
  2. custompartitioned between ethyl acetate and water
  3. washThe organic solution was washed with water (2×)
  4. customdried
  5. concentrationconcentrated
  6. customto produce a light yellow oil

出典と根拠

ORDレコード
ord-5580b2adf3214d2e9afa28f9a0cdfacb
出典データセット
uspto-grants-2015_11
特許番号
US09175042B2

反応ノート

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