Acetic Acid → 9-Methyl-5-nitroso-2,3,4,5-tetrahydro-1,5-benzothiazepine

HRID 1764845ノート

反応式

HRID 1764845 の反応式
[CH3:1][C:2]1[C:12]2[S:11][CH2:10][CH2:9][CH2:8][NH:7][C:6]=2[CH:5]=[CH:4][CH:3]=1.CC(O)=O.[N:17]([O-])=[O:18].[Na+]>O>[CH3:1][C:2]1[C:12]2[S:11][CH2:10][CH2:9][CH2:8][N:7]([N:17]=[O:18])[C:6]=2[CH:5]=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 176Acetic AcidHCID 227353879-Methyl-2,3,4,5-tetrahydro-1,5-benzothiazepineHCID 23668193Sodium Nitrite

生成物 1

HCID 227360929-Methyl-5-nitroso-2,3,4,5-tetrahydro-1,5-benzothiazepine

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
23 °C

実験手順

To a solution of 9-methyl-2,3,4,5-tetrahydro-1,5-benzothiazepine (500 mg, 2.6 mmol) and AcOH (2 mL) cooled to ˜9° C. was added a solution of NaNO2 (212 mg, 3.1 mmol) and water (1 mL) dropwise over 4 min (internal temperature<12° C.). The cooling bath was removed and the reaction was maintained at 23° C. for 2 h. It was diluted with H2O (50 mL). 9-methyl-5-nitroso-2,3,4,5-tetrahydro-1,5-benzothiazepine was obtained (470 mg, 87%) as a yellow solid after it was collected by vacuum filtration and air-dried at 23° C.

後処理

  1. customThe cooling bath was removed
  2. additionIt was diluted with H2O (50 mL)

出典と根拠

ORDレコード
ord-4e9856cac9604adaa097d14ef6e81d67
出典データセット
uspto-grants-2007_06
特許番号
USRE039679E1

反応ノート

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